#------------------------------------------------------------------------------
#$Date: 2022-05-25 00:30:41 +0200 (Wed 25 de May de 2022) $
#$Revision: 275628 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/49/7244976.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7244976
loop_
_publ_author_name
'Sugimoto, Akira'
'Kusumoto, Sotaro'
'Nakaya, Manabu'
'Sekine, Yoshihiro'
'Lindoy, Leonard F.'
'Hayami, Shinya'
_publ_section_title
;
 Modulation of the elasticity of single crystal, 1-D metal
 dimethylglyoximato complexes via solid solution effect
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00402J
_journal_year                    2022
_chemical_formula_moiety         'C8 H14 N4 O4 Pt'
_chemical_formula_sum            'C8 H14 N4 O4 Pt'
_chemical_formula_weight         425.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-03 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2744(11)
_cell_length_b                   10.6919(7)
_cell_length_c                   6.3727(4)
_cell_measurement_reflns_used    1528
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.7350
_cell_measurement_theta_min      2.4530
_cell_volume                     1108.88(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  -9.00   0.50    3.21    --    5.00  45.00 150.00  150
  2  ω     -1.00  42.00   0.50    3.21    --    5.00  45.00 150.00   86
  3  ω    -92.00 -30.00   0.50    3.21    --   -8.70  45.00  60.00  124
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137117000
_diffrn_orient_matrix_UB_12      -0.0630403000
_diffrn_orient_matrix_UB_13      0.0008341000
_diffrn_orient_matrix_UB_21      0.0412755000
_diffrn_orient_matrix_UB_22      0.0208888000
_diffrn_orient_matrix_UB_23      -0.0063503000
_diffrn_orient_matrix_UB_31      0.0024125000
_diffrn_orient_matrix_UB_32      0.0014943000
_diffrn_orient_matrix_UB_33      0.1110328000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3042
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.803
_diffrn_reflns_theta_min         2.279
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    12.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0263P)²+0.1950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                624
_reflns_number_total             761
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00402j2.cif
_cod_data_source_block           Pt(HDMG)2
_cod_database_code               7244976
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pt C N O'
_chemical_oxdiff_usercomment     100
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_diffrn_oxdiff_ac4_digest_frames
;
01558bf129a7154c19822fa075033778eb003601e17
;
_diffrn_oxdiff_ac4_digest_hkl
;
019b1de1032c46edae1731f2c8b82eeb43ecea
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
3.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
3.b Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_file
;
TITL 200728_sugi_pt2_a.res in Ibam
    200728_sugi_pt2.res
    created by SHELXL-2018/3 at 10:31:38 on 03-Feb-2022
REM Old TITL 200728_sugi_Pt2 in Iba2
REM SHELXT solution in Ibam
REM R1 0.027, Rweak 0.000, Alpha 0.013, Orientation as input
REM Formula found by SHELXT: C10 N2 O4 Pt
CELL 0.71073 16.2744 10.6919 6.3727 90 90 90
ZERR 4 0.0011 0.0007 0.0004 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O Pt
UNIT 32 56 16 16 4

L.S. 5 0 0
PLAN  5
CONF
list 4
fmap 2 53
acta
MORE -1
BOND $H
REM <olex2.extras>
REM <HklSrc "%.\\200728_sugi_Pt2.hkl">
REM </olex2.extras>

WGHT    0.026300    0.195000
FVAR       0.17273
PT1   5    0.500000    0.500000    0.500000    10.25000    0.00962    0.00944 =
         0.00785    0.00000    0.00000   -0.00019
O3    4    0.551618    0.762708    0.500000    10.50000    0.01282    0.01271 =
         0.02134    0.00000    0.00000   -0.00553
AFIX 147
H3    2    0.592883    0.725302    0.538894    10.50000   -1.50000
AFIX   0
O4    4    0.332693    0.411681    0.500000    10.50000    0.01282    0.01503 =
         0.02061    0.00000    0.00000   -0.00686
N2    3    0.378773    0.513771    0.500000    10.50000    0.01332    0.01425 =
         0.01044    0.00000    0.00000    0.00180
N1    3    0.485602    0.682045    0.500000    10.50000    0.01644    0.01052 =
         0.01295    0.00000    0.00000   -0.00229
C3    1    0.258659    0.648673    0.500000    10.50000    0.01546    0.02114 =
         0.02554    0.00000    0.00000    0.00158
PART -1
AFIX 137
H3A   2    0.237524    0.637120    0.639299    10.50000   -1.50000
H3B   2    0.232608    0.590585    0.406357    10.50000   -1.50000
H3C   2    0.247605    0.732567    0.454345    10.50000   -1.50000
AFIX   0
PART 0
C1    1    0.348620    0.626658    0.500000    10.50000    0.01637    0.01625 =
         0.00852    0.00000    0.00000    0.00253
C2    1    0.393927    0.862331    0.500000    10.50000    0.02010    0.01429 =
         0.02005    0.00000    0.00000    0.00466
PART -1
AFIX 137
H2A   2    0.404481    0.895980    0.362962    10.50000   -1.50000
H2B   2    0.428578    0.903172    0.600833    10.50000   -1.50000
H2C   2    0.337371    0.875951    0.536206    10.50000   -1.50000
AFIX   0
PART 0
C0AA  1    0.411519    0.725758    0.500000    10.50000    0.01510    0.01732 =
         0.01063    0.00000    0.00000    0.00114
HKLF 4




REM  200728_sugi_pt2_a.res in Ibam
REM wR2 = 0.0456, GooF = S = 1.111, Restrained GooF = 1.111 for all data
REM R1 = 0.0170 for 624 Fo > 4sig(Fo) and 0.0215 for all 761 data
REM 56 parameters refined using 0 restraints

END

WGHT      0.0263      0.1950

REM Highest difference peak  1.665,  deepest hole -1.304,  1-sigma level  0.158
Q1    1   0.4994  0.5192  0.6181  11.00000  0.05    1.66
Q2    1   0.5000  0.5618  0.2500  10.50000  0.05    0.79
Q3    1   0.4999  0.5965  0.5000  10.50000  0.05    0.69
Q4    1   0.4595  0.4962  0.5000  10.50000  0.05    0.60
Q5    1   0.5774  0.7241  0.5000  10.50000  0.05    0.54
;
_shelx_res_checksum              32367
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.796
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.500000 0.500000 0.500000 0.00897(10) Uani 1 4 d S T P . .
O3 O 0.55162(17) 0.7627(3) 0.500000 0.0156(6) Uani 1 2 d S T P . .
H3 H 0.592883 0.725302 0.538894 0.023 Uiso 0.5 1 calc R U P . .
O4 O 0.33269(18) 0.4117(3) 0.500000 0.0162(6) Uani 1 2 d S T P . .
N2 N 0.3788(3) 0.5138(3) 0.500000 0.0127(8) Uani 1 2 d S T P . .
N1 N 0.4856(2) 0.6820(4) 0.500000 0.0133(8) Uani 1 2 d S T P . .
C3 C 0.2587(2) 0.6487(4) 0.500000 0.0207(9) Uani 1 2 d S T P . .
H3A H 0.237524 0.637120 0.639299 0.031 Uiso 0.5 1 calc R U P A -1
H3B H 0.232608 0.590585 0.406357 0.031 Uiso 0.5 1 calc R U P A -1
H3C H 0.247605 0.732567 0.454345 0.031 Uiso 0.5 1 calc R U P A -1
C1 C 0.3486(3) 0.6267(4) 0.500000 0.0137(8) Uani 1 2 d S T P . .
C2 C 0.3939(3) 0.8623(3) 0.500000 0.0181(9) Uani 1 2 d S T P . .
H2A H 0.404481 0.895980 0.362962 0.027 Uiso 0.5 1 calc R U P B -1
H2B H 0.428578 0.903172 0.600833 0.027 Uiso 0.5 1 calc R U P B -1
H2C H 0.337371 0.875951 0.536206 0.027 Uiso 0.5 1 calc R U P B -1
C0AA C 0.4115(2) 0.7258(4) 0.500000 0.0143(8) Uani 1 2 d S T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.00962(13) 0.00944(14) 0.00785(14) 0.000 0.000 -0.00019(7)
O3 0.0128(13) 0.0127(13) 0.0213(16) 0.000 0.000 -0.0055(12)
O4 0.0128(14) 0.0150(14) 0.0206(16) 0.000 0.000 -0.0069(12)
N2 0.0133(19) 0.0142(17) 0.0104(18) 0.000 0.000 0.0018(12)
N1 0.0164(17) 0.0105(18) 0.0130(19) 0.000 0.000 -0.0023(13)
C3 0.015(2) 0.021(2) 0.026(2) 0.000 0.000 0.0016(16)
C1 0.016(2) 0.0162(18) 0.0085(18) 0.000 0.000 0.0025(16)
C2 0.020(2) 0.0143(18) 0.020(2) 0.000 0.000 0.0047(15)
C0AA 0.015(2) 0.0173(19) 0.0106(19) 0.000 0.000 0.0011(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pt1 Pt1 Pt1 180.0 7_545 7_546 ?
N2 Pt1 Pt1 90.0 9_666 7_545 ?
N2 Pt1 Pt1 90.0 . 7_546 ?
N2 Pt1 Pt1 90.0 9_666 7_546 ?
N2 Pt1 Pt1 90.0 . 7_545 ?
N2 Pt1 N2 180.0 . 9_666 ?
N1 Pt1 Pt1 90.0 . 7_546 ?
N1 Pt1 Pt1 90.0 . 7_545 ?
N1 Pt1 Pt1 90.0 9_666 7_545 ?
N1 Pt1 Pt1 90.0 9_666 7_546 ?
N1 Pt1 N2 78.87(12) 9_666 9_666 ?
N1 Pt1 N2 78.87(12) . . ?
N1 Pt1 N2 101.13(12) 9_666 . ?
N1 Pt1 N2 101.13(12) . 9_666 ?
N1 Pt1 N1 180.0 . 9_666 ?
H3 O3 H3 35.2 . 10_556 ?
N1 O3 H3 109.5(10) . 10_556 ?
N1 O3 H3 109.5 . . ?
O4 N2 Pt1 120.2(2) . . ?
C1 N2 Pt1 116.4(3) . . ?
C1 N2 O4 123.4(4) . . ?
O3 N1 Pt1 121.9(3) . . ?
C0AA N1 Pt1 118.1(3) . . ?
C0AA N1 O3 120.1(4) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
N2 C1 C3 121.3(4) . . ?
N2 C1 C0AA 113.9(4) . . ?
C0AA C1 C3 124.9(3) . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C0AA C2 H2A 109.5 . . ?
C0AA C2 H2B 109.5 . . ?
C0AA C2 H2C 109.5 . . ?
N1 C0AA C1 112.8(3) . . ?
N1 C0AA C2 122.3(4) . . ?
C1 C0AA C2 124.9(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 Pt1 3.1864(2) 7_546 ?
Pt1 Pt1 3.1864(2) 7_545 ?
Pt1 N2 1.978(4) 9_666 ?
Pt1 N2 1.978(4) . ?
Pt1 N1 1.960(4) . ?
Pt1 N1 1.960(4) 9_666 ?
O3 H3 0.82(4) 10_556 ?
O3 H3 0.8200 . ?
O3 N1 1.378(4) . ?
O4 N2 1.324(4) . ?
N2 C1 1.303(5) . ?
N1 C0AA 1.293(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C1 1.483(5) . ?
C1 C0AA 1.473(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 C0AA 1.488(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pt1 N2 C1 C3 180.0 . . . . ?
Pt1 N2 C1 C0AA 0.0 . . . . ?
Pt1 N1 C0AA C1 0.0 . . . . ?
Pt1 N1 C0AA C2 180.0 . . . . ?
O3 N1 C0AA C1 180.0 . . . . ?
O3 N1 C0AA C2 0.0 . . . . ?
O4 N2 C1 C3 0.0 . . . . ?
O4 N2 C1 C0AA 180.0 . . . . ?
N2 C1 C0AA N1 0.0 . . . . ?
N2 C1 C0AA C2 180.0 . . . . ?
C3 C1 C0AA N1 180.0 . . . . ?
C3 C1 C0AA C2 0.0 . . . . ?
