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_4346984
_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 H40 B4 N2 O6 Sn, C7 H8'
_chemical_formula_sum            'C43 H48 B4 N2 O6 Sn'
_chemical_formula_weight         850.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 102.792(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1391(9)
_cell_length_b                   11.9130(6)
_cell_length_c                   17.5390(5)
_cell_measurement_reflns_used    20422
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2065.9(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20380
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.060
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 3486 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8933
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+1.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.875
_reflns_number_gt                8245
_reflns_number_total             8933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02505_si_002.cif
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4346984