N→Sn-Coordinated Stannaoxidoborates Containing a SnB4O6 Unit.
Mairychová, Barbora; Kityk, I. V.; Maciag, Artur; Bureš, Filip; Klikar, Milan; Růžička, Aleš; Dostál, Libor; Jambor, Roman; Inorganic chemistry 55 (2016) 1587–1594; doi:10.1021/acs.inorgchem.5b02505

data_4346985
_publ_section_title
;
 N\\rightarrow Sn-Coordinated Stannaoxidoborates Containing a SnB4O6 Unit.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1587
_journal_page_last               1594
_journal_paper_doi               10.1021/acs.inorgchem.5b02505
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H36 B4 Br4 N2 O6 Sn, C7 H8'
_chemical_formula_sum            'C43 H44 B4 Br4 N2 O6 Sn'
_chemical_formula_weight         1166.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0820(10)
_cell_length_b                   15.0270(6)
_cell_length_c                   22.8241(17)
_cell_measurement_reflns_used    31424
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      1
_cell_volume                     4829.8(5)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31284
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.800
_diffrn_reflns_theta_min         1.784
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.884
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2919 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0213P)^2^+8.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                7501
_reflns_number_total             9051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02505_si_002.cif
_cod_data_source_block           compound7
_cod_database_code               4346985