#------------------------------------------------------------------------------
#$Date: 2019-07-03 12:24:39 +0200 (Wed 03 de Jul de 2019) $
#$Revision: 216710 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/63/1546341.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_1546341
loop_
_publ_author_name
'Gair, Joe J.'
'Haines, Brandon E.'
'Filatov, Alexander S.'
'Musaev, D. G.'
'Lewis, Jared C.'
_publ_section_title
;
 Mono-N-Protected Amino Acid Ligands Stabilize Dimeric Palladium(II)
 Complexes of Importance to C-H Functionalization
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01674C
_journal_year                    2017
_chemical_formula_moiety         'Cl3 Pd, C2 H8 N'
_chemical_formula_sum            'C2 H8 Cl3 N Pd'
_chemical_formula_weight         258.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8831(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6908(5)
_cell_length_b                   13.0776(8)
_cell_length_c                   7.1107(4)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.72
_cell_measurement_theta_min      3.07
_cell_volume                     715.09(8)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17218
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.747
_diffrn_reflns_theta_min         3.073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.603
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0359 after correction.
The Ratio of minimum to maximum transmission is 0.8080.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         1435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0137
_refine_ls_R_factor_gt           0.0115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0085P)²+0.5992P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0247
_refine_ls_wR_factor_ref         0.0253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1339
_reflns_number_total             1435
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc01674c6.cif
_cod_data_source_block           complex_S5_1
_cod_depositor_comments
;

2019-06-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C4 H16 Cl6 N2 Pd2'
_cod_original_formula_weight         517.69
_cod_original_formula_moiety         'Cl6 Pd2, 2(C2 H8 N)'
_cod_original_formula_units_Z            2
_cod_database_code               1546341
_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.
;
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.392
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_file
;
TITL 0306
    0306.res
    created by SHELXL-2016/6 at 15:15:50 on 28-Dec-2016
CELL 0.71073 7.6908 13.0776 7.1107 90 90.8831 90
ZERR 2 0.0005 0.0008 0.0004 0 0.0014 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cl N Pd
UNIT 8 32 12 4 4

L.S. 15
PLAN  10
SIZE 0.11 0.12 0.32
TEMP -173
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\03060_Gair04_monoclinic_C.hkl">
REM </olex2.extras>

WGHT    0.008500    0.599200
FVAR       0.12762
PD1   5    0.500000    0.500000    0.500000    10.50000    0.01095    0.00904 =
         0.00678    0.00039    0.00067   -0.00014
CL2   3    0.500000    0.612542    0.750000    10.50000    0.02035    0.01051 =
         0.00829    0.00000    0.00062    0.00000
CL1   3    0.753170    0.426968    0.614080    11.00000    0.01353    0.01553 =
         0.01286    0.00015   -0.00098    0.00240
N1    4    1.000000    0.374171    0.250000    10.50000    0.01488    0.01309 =
         0.01325    0.00000    0.00062    0.00000
H1    2    1.073200    0.413237    0.203056    11.00000    0.02419
C2    1    1.083620    0.310404    0.399082    11.00000    0.02012    0.01770 =
         0.01819    0.00307   -0.00124    0.00222
AFIX 137
H2A   2    1.171901    0.266390    0.342874    11.00000   -1.50000
H2B   2    0.995356    0.267911    0.459059    11.00000   -1.50000
H2C   2    1.138704    0.354890    0.493552    11.00000   -1.50000
AFIX   0
HKLF 4




REM  0306
REM R1 =  0.0115 for    1339 Fo > 4sig(Fo)  and  0.0137 for all    1435 data
REM     40 parameters refined using      0 restraints

END

WGHT      0.0083      0.6194

REM Highest difference peak  0.443,  deepest hole -0.534,  1-sigma level  0.072
Q1    1   1.2416  0.4336  0.3898  11.00000  0.05    0.44
Q2    1   0.5000  0.3921  0.7500  10.50000  0.05    0.43
Q3    1   0.9591  0.3476  0.1911  11.00000  0.05    0.37
Q4    1   1.0000  0.2944  0.2500  10.50000  0.05    0.37
Q5    1   0.5369  0.4804  0.4779  11.00000  0.05    0.30
Q6    1   0.5145  0.5859  0.8185  11.00000  0.05    0.27
Q7    1   0.7470  0.3818  0.6914  11.00000  0.05    0.26
Q8    1   0.4222  0.5868  0.7785  11.00000  0.05    0.25
Q9    1   0.6397  0.4527  0.5537  11.00000  0.05    0.25
Q10   1   0.5622  0.5595  0.7506  11.00000  0.05    0.23
;
_shelx_res_checksum              23477
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Pd1 Pd 0.500000 0.500000 0.500000 0.00892(3) Uani 1 2 d S T P
Cl2 Cl 0.500000 0.61254(2) 0.750000 0.01304(6) Uani 1 2 d S T P
Cl1 Cl 0.75317(3) 0.42697(2) 0.61408(3) 0.01399(5) Uani 1 1 d . . .
N1 N 1.000000 0.37417(10) 0.250000 0.0137(2) Uani 1 2 d S T P
H1 H 1.0732(19) 0.4132(12) 0.203(2) 0.024(4) Uiso 1 1 d . . .
C2 C 1.08362(14) 0.31040(9) 0.39908(16) 0.01868(19) Uani 1 1 d . . .
H2A H 1.171901 0.266390 0.342874 0.028 Uiso 1 1 calc GR . .
H2B H 0.995356 0.267911 0.459059 0.028 Uiso 1 1 calc GR . .
H2C H 1.138704 0.354890 0.493552 0.028 Uiso 1 1 calc GR . .
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
Pd1 0.01095(4) 0.00904(4) 0.00678(4) 0.00039(3) 0.00067(3) -0.00014(3)
Cl2 0.02035(15) 0.01051(13) 0.00829(12) 0.000 0.00062(10) 0.000
Cl1 0.01353(9) 0.01553(10) 0.01286(9) 0.00015(8) -0.00098(7) 0.00240(8)
N1 0.0149(5) 0.0131(5) 0.0132(5) 0.000 0.0006(4) 0.000
C2 0.0201(5) 0.0177(5) 0.0182(5) 0.0031(4) -0.0012(4) 0.0022(4)
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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 '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
Cl2 Pd1 Cl2 180.0 . 5_666
Cl1 Pd1 Cl2 90.182(7) 5_666 5_666
Cl1 Pd1 Cl2 90.183(7) . .
Cl1 Pd1 Cl2 89.817(7) . 5_666
Cl1 Pd1 Cl2 89.818(7) 5_666 .
Cl1 Pd1 Cl1 180.0 . 5_666
Pd1 Cl2 Pd1 100.756(13) . 2_656
H1 N1 H1 104(2) . 2_755
C2 N1 H1 110.0(11) . .
C2 N1 H1 110.2(11) . 2_755
C2 N1 H1 110.2(11) 2_755 .
C2 N1 H1 110.0(11) 2_755 2_755
C2 N1 C2 111.79(12) . 2_755
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl2 2.3079(2) .
Pd1 Cl2 2.3079(2) 5_666
Pd1 Cl1 2.3049(3) .
Pd1 Cl1 2.3049(3) 5_666
N1 H1 0.834(15) 2_755
N1 H1 0.834(15) .
N1 C2 1.4872(13) .
N1 C2 1.4872(13) 2_755
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
