#------------------------------------------------------------------------------
#$Date: 2020-06-05 11:54:52 +0200 (vie 05 de jun de 2020) $
#$Revision: 252716 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/62/7126250.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_7126250
loop_
_publ_author_name
'Wu, Qi'
'Liu, Xian'
'Du, Yeshuang'
'Teng, Chunlin'
'Liang, Fei'
_publ_section_title
;
 Nonlinear organic-inorganic halide hybrids containing unprecedented
 linear [MIX₂]⁻ coordination units and
 quasi-two-dimensional lone pairs.
;
_journal_issue                   36
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4894
_journal_page_last               4897
_journal_paper_doi               10.1039/d0cc01532f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(Cl Ga0.5), C4 H12 N'
_chemical_formula_sum            'C4 H12 Cl2 Ga N'
_chemical_formula_weight         214.77
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-08 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2755(6)
_cell_length_b                   9.2755(6)
_cell_length_c                   5.8368(4)
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      3.11
_cell_volume                     502.17(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2057
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.447
_diffrn_reflns_theta_min         3.491
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 12002 reflections, Rint = 0.1025
 (7397 with I > 3sig(I), Rint = 0.0846)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.208
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details
;
 Flack x determined using 179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0744
_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)+(0.1414P)²+1.0876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.650
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                542
_reflns_number_total             566
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc01532f2.cif
_cod_data_source_block           2_0m_4
_cod_depositor_comments
'Adding full bibliography for 7126250--7126251.cif.'
_cod_original_cell_volume        502.17(7)
_cod_database_code               7126250
_shelx_shelxl_version_number     2016/6
_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   0.681
_shelx_estimated_absorpt_t_min   0.568
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.44(17)
 0.56(17)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c)
;
_shelx_res_file
;
TITL 2_0m_4 in P-421m #113
    2_0m_4.res
    created by SHELXL-2016/6 at 20:56:59 on 02-Aug-2019
REM reset to P-421m #113
CELL 0.71073 9.2755 9.2755 5.8368 90 90 90
ZERR 2 0.0006 0.0006 0.0004 0 0 0
LATT -1
SYMM +Y,-X,-Z
SYMM -X,-Y,+Z
SYMM -Y,+X,-Z
SYMM 0.5+X,0.5-Y,-Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC C H Cl Ga N
UNIT 8 24 4 2 2

L.S. 4 0 0
PLAN  20
SIZE 0.12 0.16 0.18
TEMP -100.15
BOND
fmap 2 50
acta
TWIN 0 1 0 -1 0 0 0 0 1 2
OMIT -2 53
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\2_0m_4.hkl">
REM </olex2.extras>

WGHT    0.141400    1.087600
BASF   0.56377
FVAR       1.23451
GA1   4    0.000000    0.500000   -0.107406    10.25000    0.03910    0.03910 =
         0.03713    0.00000    0.00000   -0.01393
CL1   3    0.193852    0.306148   -0.106513    10.50000    0.07999    0.07999 =
         0.08512   -0.00096    0.00096   -0.00580
N1    5    0.000000    0.000000    0.500000    10.25000    0.07577    0.07577 =
         0.06031    0.00000    0.00000    0.00000
C1    1    0.061033    0.114142    0.353275    11.00000    0.08224    0.07357 =
         0.08879    0.00026   -0.00008   -0.00970
AFIX 137
H1A   2    0.146739    0.077269    0.274493    11.00000   -1.50000
H1B   2    0.087825    0.197127    0.448074    11.00000   -1.50000
H1C   2   -0.010908    0.143882    0.239754    11.00000   -1.50000
AFIX   0
HKLF 4




REM  2_0m_4 in P-421m #113
REM R1 =  0.0744 for     542 Fo > 4sig(Fo)  and  0.0781 for all     566 data
REM     24 parameters refined using      0 restraints

END

WGHT      0.1414      1.0876

REM Highest difference peak  1.208,  deepest hole -1.177,  1-sigma level  0.195
Q1    1   0.0000  0.5000  0.3784  10.25000  0.05    0.95
Q2    1   0.0000  0.5000  0.2878  10.25000  0.05    0.93
Q3    1   0.3080  0.1920  0.1076  10.50000  0.05    0.54
Q4    1   0.3439  0.1561  0.2822  10.50000  0.05    0.46
Q5    1   0.0000  0.5000 -0.3377  10.25000  0.05    0.43
Q6    1   0.2854  0.3487  0.0461  11.00000  0.05    0.41
Q7    1   0.3037  0.1963 -0.3063  10.50000  0.05    0.38
Q8    1   0.0213  0.2147  0.1999  11.00000  0.05    0.35
Q9    1   0.1982  0.1376  0.1347  11.00000  0.05    0.35
Q10   1   0.3392  0.2735 -0.0375  11.00000  0.05    0.34
Q11   1   0.0154  0.2574  0.1486  11.00000  0.05    0.33
Q12   1   0.0624  0.5624 -0.4821  10.50000  0.05    0.32
Q13   1   0.0663  0.1851  0.1768  11.00000  0.05    0.32
Q14   1   0.1003  0.0412  0.1502  11.00000  0.05    0.32
Q15   1   0.3184  0.3550 -0.1632  11.00000  0.05    0.29
Q16   1  -0.0012  0.3857  0.4976  11.00000  0.05    0.29
Q17   1   0.2405  0.4254  0.0094  11.00000  0.05    0.27
Q18   1  -0.0008  0.0874  0.1233  11.00000  0.05    0.27
Q19   1  -0.0884  0.0955  0.3574  11.00000  0.05    0.27
Q20   1   0.0605  0.2587 -0.0420  11.00000  0.05    0.26
;
_shelx_res_checksum              4844
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
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
Ga1 Ga 0.000000 0.500000 -0.1074(3) 0.0384(8) Uani 1 4 d S T P . .
Cl1 Cl 0.1939(5) 0.3061(5) -0.1065(11) 0.0817(18) Uani 1 2 d S T P . .
N1 N 0.000000 0.000000 0.500000 0.071(6) Uani 1 4 d S T P . .
C1 C 0.061(2) 0.1141(19) 0.353(3) 0.082(5) Uani 1 1 d . . . . .
H1A H 0.146739 0.077269 0.274493 0.122 Uiso 1 1 calc GR . . . .
H1B H 0.087825 0.197127 0.448074 0.122 Uiso 1 1 calc GR . . . .
H1C H -0.010908 0.143882 0.239754 0.122 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
Ga1 0.0391(9) 0.0391(9) 0.0371(12) 0.000 0.000 -0.0139(10)
Cl1 0.080(2) 0.080(2) 0.085(4) -0.001(2) 0.001(2) -0.006(3)
N1 0.076(9) 0.076(9) 0.060(13) 0.000 0.000 0.000
C1 0.082(10) 0.074(10) 0.089(13) 0.000(10) 0.000(9) -0.010(8)
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'
Ga Ga 0.2307 1.6083 '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'
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
Cl1 Ga1 Cl1 179.8(3) 3_565 . ?
C1 N1 C1 109.7(7) . 2_556 ?
C1 N1 C1 109.0(14) . 3 ?
C1 N1 C1 109.7(7) 3 4_556 ?
C1 N1 C1 109.0(14) 2_556 4_556 ?
C1 N1 C1 109.7(7) 3 2_556 ?
C1 N1 C1 109.7(7) . 4_556 ?
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
Ga1 Cl1 2.543(7) 3_565 ?
Ga1 Cl1 2.543(7) . ?
N1 C1 1.475(17) . ?
N1 C1 1.475(17) 3 ?
N1 C1 1.475(17) 2_556 ?
N1 C1 1.475(17) 4_556 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.44(17)
2 0.56(17)
