Crystal structure of 12-chloro-5,6,7,12-tetrahydrodibenzo[c,f][1,5]oxastibocine, C14H12ClOSb
Tan, Nianyuan; Lan, Donghui; Wu, Shuisheng; Au, Chak-Tong; Yi, Bing; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 679–681; doi:10.1515/ncrs-2018-0006

data_8106259
_publ_section_title
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 Crystal structure of
 12-chloro-5,6,7,12-tetrahydrodibenzo[c,f][1,5]oxastibocine, C14H12ClOSb
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              679
_journal_page_last               681
_journal_paper_doi               10.1515/ncrs-2018-0006
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C14 H12 Cl O Sb'
_chemical_formula_sum            'C14 H12 Cl O Sb'
_chemical_formula_weight         353.44
_chemical_name_systematic
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12-Chloro-5,6,7,12-tetrahydrodibenzo[c,f][1,5]oxastibocine 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.823(3)
_cell_angle_beta                 90.394(3)
_cell_angle_gamma                108.307(2)
_cell_formula_units_Z            4
_cell_length_a                   9.3453(14)
_cell_length_b                   10.9826(16)
_cell_length_c                   13.303(2)
_cell_measurement_reflns_used    2011
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.277
_cell_measurement_theta_min      4.922
_cell_volume                     1296.0(3)
_computing_cell_refinement       'SAINT  (Bruker, 2004)'
_computing_data_collection       'SMART  (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenberg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6765
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0969
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.633
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.183
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4729
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+2.3779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                3750
_reflns_number_total             4729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2018-0006_suppl.cif
_cod_data_source_block           cd
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8106259
_publcif_funding_html
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