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_4002984
_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         '0.25(Br16 Cs4 Sn4), 2(C0.5 H3 N1.5)'
_chemical_formula_sum            'C H6 Br4 Cs N3 Sn'
_chemical_formula_weight         631.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.0112(10)
_cell_length_b                   11.5363(18)
_cell_length_c                   17.342(3)
_cell_measurement_reflns_used    2457
_cell_measurement_temperature    250
_cell_measurement_theta_max      30.634
_cell_measurement_theta_min      2.349
_cell_volume                     1202.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      250
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.436
_diffrn_reflns_theta_min         2.120
_exptl_absorpt_coefficient_mu    18.348
_exptl_absorpt_correction_T_max  0.3400
_exptl_absorpt_correction_T_min  0.1656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1371 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.4871. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_recrystallization_method
'crystallized from hydrobromic acid (HBr, 48% water solution)'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.656
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.00437(17)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         1079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                947
_reflns_number_total             1079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b00038_si_003.cif
_cod_data_source_block           imma
_cod_database_code               4002984
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.137
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Sof(Br3B)=0.25*(1-FVAR(2))
 Sof(Br3A)=0.25*FVAR(2)
 Fixed Sof: H1A(0.25) H1B(0.25)
3.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_shelx_res_checksum              89653
_shelx_hkl_checksum              20386
_olex2_submission_special_instructions 'No special instructions were received'