Guanidinium and Mixed Cesium-Guanidinium Tin(II) Bromides: Effects of Quantum Confinement and Out-of-Plane Octahedral Tilting.
Nazarenko, Olga; Kotyrba, Martin R.; Yakunin, Sergii; Wörle, Michael; Benin, Bogdan M.; Rainò, Gabriele; Krumeich, Frank; Kepenekian, Mikaël; Even, Jacky; Katan, Claudine; Kovalenko, Maksym V.; Chemistry of materials : a publication of the American Chemical Society 31 (2019) 2121–2129; doi:10.1021/acs.chemmater.9b00038

data_4002983
_publ_section_title
;
 Guanidinium and Mixed Cesium-Guanidinium Tin(II) Bromides: Effects of
 Quantum Confinement and Out-of-Plane Octahedral Tilting.
;
_journal_issue                   6
_journal_name_full
'Chemistry of materials : a publication of the American Chemical Society'
_journal_page_first              2121
_journal_page_last               2129
_journal_paper_doi               10.1021/acs.chemmater.9b00038
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         '0.5(Br8 Sn2), 2(C H6 N3)'
_chemical_formula_sum            'C2 H12 Br4 N6 Sn'
_chemical_formula_weight         558.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-25 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.082(3)
_cell_length_b                   8.3226(6)
_cell_length_c                   10.4238(8)
_cell_measurement_reflns_used    5575
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.855
_cell_measurement_theta_min      2.330
_cell_volume                     2783.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker SMART CCD 1K area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29756
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.026
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.296
_exptl_absorpt_correction_T_max  0.1291
_exptl_absorpt_correction_T_min  0.0651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1579 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.5043. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.666
_exptl_crystal_description       needle
_exptl_crystal_F_000             2048
_exptl_crystal_recrystallization_method
'crystallized from hydrobromic acid (48 percent water solution)'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_coef       0.00185(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         7393
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0348
_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/[\s^2^(Fo^2^)+(0.0287P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5460
_reflns_number_total             7393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b00038_si_001.cif
_cod_data_source_block           pna21
_cod_original_formula_sum        'C2 H12 N6 Sn Br4 '
_cod_database_code               4002983
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.109
_shelx_estimated_absorpt_t_min   0.093
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(2)
 0.10(2)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
3.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B), N10(H10A,H10B), N11(H11A,H11B),
 N12(H12A,H12B)
;
_shelx_res_checksum              50758
_shelx_hkl_checksum              6927
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'