#------------------------------------------------------------------------------
#$Date: 2019-11-22 21:56:14 +0100 (vie 22 de nov de 2019) $
#$Revision: 231503 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/32/4003299.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_4003299
loop_
_publ_author_name
'Dang, Yangyang'
'Zhong, Cheng'
'Zhang, Guodong'
'Ju, Dianxing'
'Wang, Lei'
'Xia, Shengqing'
'Xia, Haibing'
'Tao, Xutang'
_publ_section_title
;
 Crystallographic Investigations into Properties of Acentric Hybrid
 Perovskite Single Crystals NH(CH3)3SnX3 (X = Cl, Br)
;
_journal_issue                   19
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6968
_journal_paper_doi               10.1021/acs.chemmater.6b02653
_journal_volume                  28
_journal_year                    2016
_chemical_formula_sum            'C3 H10 Cl3 N Sn'
_chemical_formula_weight         285.16
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.172(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.370(7)
_cell_length_b                   8.267(7)
_cell_length_c                   12.355(10)
_cell_measurement_reflns_used    1615
_cell_measurement_temperature    260
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.29
_cell_volume                     956.4(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      260
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2135
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    3.431
_exptl_absorpt_correction_T_max  0.7254
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.380
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.325
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(14)
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1445
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1264P)²+30.6032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2178
_refine_ls_wR_factor_ref         0.2186
_reflns_number_gt                1404
_reflns_number_total             1445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm6b02653_si_002.cif
_cod_data_source_block           x1
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4003299
loop_
_symmetry_equiv_pos_as_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'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 1.0187(6) 0.9604(4) 0.7412(6) 0.0306(8) Uani 0.50 1 d P
Sn2 Sn 1.020(2) 0.9570(5) 0.7347(15) 0.134(5) Uani 0.50 1 d P
Cl1 Cl 1.0471(8) 0.9778(7) 0.9399(6) 0.0677(17) Uani 1 1 d .
Cl2 Cl 1.1988(9) 0.7428(9) 0.7378(6) 0.081(2) Uani 1 1 d .
Cl3 Cl 0.8270(6) 0.7472(10) 0.7525(7) 0.078(2) Uani 1 1 d .
N1 N 0.530(2) 1.0654(19) 0.9612(15) 0.051(4) Uani 1 1 d .
C1 C 0.494(4) 0.911(3) 0.903(3) 0.107(12) Uani 1 1 d .
C2 C 0.429(3) 1.100(5) 1.049(3) 0.099(11) Uani 1 1 d .
C3 C 0.684(5) 1.070(5) 0.999(6) 0.19(3) Uani 1 1 d .
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
Sn1 0.0185(11) 0.0377(17) 0.0358(18) 0.0093(18) 0.0043(8) -0.0002(14)
Sn2 0.349(13) 0.030(2) 0.022(3) 0.008(2) 0.002(3) 0.013(4)
Cl1 0.105(5) 0.054(3) 0.044(3) -0.002(2) 0.005(3) 0.006(3)
Cl2 0.144(7) 0.048(3) 0.051(4) 0.003(3) 0.011(4) 0.013(4)
Cl3 0.037(3) 0.074(4) 0.123(7) 0.012(4) 0.000(3) -0.007(3)
N1 0.078(12) 0.030(7) 0.043(8) 0.005(6) -0.002(8) -0.007(6)
C1 0.16(3) 0.032(11) 0.13(3) -0.051(16) -0.01(2) -0.009(15)
C2 0.069(19) 0.10(2) 0.13(3) -0.01(2) 0.05(2) -0.019(16)
C3 0.13(3) 0.08(2) 0.33(8) 0.10(4) -0.15(5) -0.03(2)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
Cl2 Sn1 Cl1 90.7(3)
Cl2 Sn1 Cl3 88.9(2)
Cl1 Sn1 Cl3 92.0(4)
Cl2 Sn2 Cl1 89.5(6)
Cl2 Sn2 Cl3 89.6(3)
Cl1 Sn2 Cl3 90.3(6)
Sn2 Cl1 Sn1 0.7(5)
Sn2 Cl2 Sn1 1.9(6)
Sn2 Cl3 Sn1 1.9(6)
C3 N1 C2 113(4)
C3 N1 C1 111(3)
C2 N1 C1 112(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn1 Cl2 2.468(10)
Sn1 Cl1 2.463(12)
Sn1 Cl3 2.524(8)
Sn2 Cl2 2.438(17)
Sn2 Cl1 2.543(16)
Sn2 Cl3 2.521(19)
N1 C3 1.50(4)
N1 C2 1.49(4)
N1 C1 1.50(3)
