#------------------------------------------------------------------------------
#$Date: 2020-06-05 12:54:52 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252716 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/62/7126251.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_7126251
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 In0.5), C4 H12 N'
_chemical_formula_sum            'C4 H12 Cl2 In N'
_chemical_formula_weight         259.87
_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     iterative
_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                   9.28070(10)
_cell_length_b                   9.28070(10)
_cell_length_c                   5.8414(2)
_cell_measurement_reflns_used    4040
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      4.91
_cell_volume                     503.128(19)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.971
_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       -7
_diffrn_reflns_number            5724
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         4.912
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 218 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.16(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0152
_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)+(0.0263P)²+0.0313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0416
_reflns_Friedel_coverage         0.663
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                556
_reflns_number_total             557
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc01532f2.cif
_cod_data_source_block           wu_3
_cod_depositor_comments
'Adding full bibliography for 7126250--7126251.cif.'
_cod_original_cell_volume        503.13(2)
_cod_database_code               7126251
_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   0.729
_shelx_estimated_absorpt_t_min   0.632
_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:
 C1(H1A,H1B,H1C)
;
_shelx_res_file
;
TITL wu_3 in P-421m #113
    wu_3.res
    created by SHELXL-2016/6 at 11:37:33 on 03-Aug-2019
REM reset to P-421m #113
CELL 0.71073 9.2807 9.2807 5.8414 90 90 90
ZERR 2 0.0001 0.0001 0.0002 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 In N
UNIT 8 24 4 2 2

L.S. 4 0 0
PLAN  5
SIZE 0.12 0.14 0.18
TEMP -100.15
fmap 2 53
acta
OMIT -2 53
OMIT 0 2 1
REM <olex2.extras>
REM <HklSrc "%.\\wu_3.hkl">
REM </olex2.extras>

WGHT    0.026300    0.031300
FVAR       1.21622
IN1   4    1.500000    0.000000   -0.607467    10.25000    0.03863    0.03863 =
         0.03040    0.00000    0.00000    0.01258
CL1   3    1.305779   -0.194221   -0.606575    10.50000    0.04909    0.04909 =
         0.04534    0.00100    0.00100    0.00649
N1    5    1.000000    0.000000    0.000000    10.25000    0.04237    0.04237 =
         0.03156    0.00000    0.00000    0.00000
C1    1    1.113090   -0.067023   -0.148109    11.00000    0.04914    0.04809 =
         0.04459   -0.00041    0.00777    0.00437
AFIX 137
H1A   2    1.069811   -0.143813   -0.240486    11.00000   -1.50000
H1B   2    1.189306   -0.107602   -0.051534    11.00000   -1.50000
H1C   2    1.154253    0.006430   -0.249352    11.00000   -1.50000
AFIX   0
HKLF 4




REM  wu_3 in P-421m #113
REM R1 =  0.0152 for     556 Fo > 4sig(Fo)  and  0.0152 for all     557 data
REM     23 parameters refined using      0 restraints

END

WGHT      0.0263      0.0313

REM Highest difference peak  0.177,  deepest hole -0.375,  1-sigma level  0.053
Q1    1   1.3596 -0.0422 -0.6069  11.00000  0.05    0.18
Q2    1   1.4020  0.0022 -0.4197  11.00000  0.05    0.16
Q3    1   1.5087  0.1313 -0.6117  11.00000  0.05    0.16
Q4    1   1.3955  0.0054 -0.7991  11.00000  0.05    0.15
Q5    1   1.3401 -0.0703 -0.6007  11.00000  0.05    0.15
;
_shelx_res_checksum              48027
_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
In1 In 1.500000 0.000000 -0.60747(5) 0.03588(16) Uani 1 4 d S T P . .
Cl1 Cl 1.30578(9) -0.19422(9) -0.60658(19) 0.0478(3) Uani 1 2 d S T P . .
N1 N 1.000000 0.000000 0.000000 0.0388(9) Uani 1 4 d S T P . .
C1 C 1.1131(3) -0.0670(4) -0.1481(6) 0.0473(7) Uani 1 1 d . . . . .
H1A H 1.069811 -0.143813 -0.240486 0.071 Uiso 1 1 calc GR . . . .
H1B H 1.189306 -0.107602 -0.051534 0.071 Uiso 1 1 calc GR . . . .
H1C H 1.154253 0.006430 -0.249352 0.071 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
In1 0.03863(18) 0.03863(18) 0.0304(2) 0.000 0.000 0.01258(16)
Cl1 0.0491(3) 0.0491(3) 0.0453(6) 0.0010(3) 0.0010(3) 0.0065(4)
N1 0.0424(13) 0.0424(13) 0.032(2) 0.000 0.000 0.000
C1 0.0491(16) 0.0481(16) 0.0446(18) -0.0004(15) 0.0078(15) 0.0044(13)
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'
In In -0.7276 1.3100 '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 In1 Cl1 179.77(5) . 3_855 ?
C1 N1 C1 109.55(14) 4_645 . ?
C1 N1 C1 109.55(14) 2_665 . ?
C1 N1 C1 109.55(14) 4_645 3_755 ?
C1 N1 C1 109.3(3) 3_755 . ?
C1 N1 C1 109.3(3) 4_645 2_665 ?
C1 N1 C1 109.55(14) 3_755 2_665 ?
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
In1 Cl1 2.5491(12) . ?
In1 Cl1 2.5491(12) 3_855 ?
N1 C1 1.496(3) 2_665 ?
N1 C1 1.496(3) 3_755 ?
N1 C1 1.496(3) . ?
N1 C1 1.496(3) 4_645 ?
