Synthesis of Distibiranes and Azadistibiranes by Cycloaddition Reactions of Distibenes with Diazomethanes and Azides
Weinert, Hanns Micha; Wölper, Christoph; Schulz, Stephan; Chemical Science  (2022) –; doi:10.1039/D2SC00314G

data_1566531
_publ_section_title
;
 Synthesis of Distibiranes and Azadistibiranes by Cycloaddition Reactions
 of Distibenes with Diazomethanes and Azides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00314G
_journal_year                    2022
_chemical_formula_sum            'C72.5 H102 F3 Ga2 N7 Sb2'
_chemical_formula_weight         1511.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                102.129(2)
_cell_angle_beta                 92.993(2)
_cell_angle_gamma                98.869(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6581(5)
_cell_length_b                   12.7136(6)
_cell_length_c                   27.5744(13)
_cell_measurement_reflns_used    9083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.43
_cell_measurement_theta_min      2.49
_cell_volume                     3595.5(3)
_computing_cell_refinement       'BRUKER APEX3(v2019.1-0)'
_computing_data_collection       'BRUKER APEX3(v2019.1-0)'
_computing_data_reduction        'BRUKER APEX3(v2019.1-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'BRUKER APEX3(v2019.1-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/QUEEN'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            190515
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.683
_diffrn_reflns_theta_min         0.758
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.126
_refine_diff_density_max         2.725
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1250
_refine_ls_number_reflns         28194
_refine_ls_number_restraints     2926
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0400P)^2^+11.3395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21619
_reflns_number_total             28194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00314g2.cif
_cod_data_source_block           mw_125_5m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3595.4(3)
_cod_original_formula_sum        'C72.50 H102 F3 Ga2 N7 Sb2'
_cod_database_code               1566531
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.584
_shelx_estimated_absorpt_t_max   0.830
_shelx_res_checksum              43433
_shelx_hkl_checksum              96098