Paddlewheel 1,2,4-diazaphospholide dibismuthanes with very short bismuth-bismuth single bonds
Minggang Zhao; Lixia Wang; Pangpang Li; Xiang Zhang; Ying Yang; Wenjun Zheng; Chem.Commun. 51 (2015) 16184–; doi:10.1039/C5cc07064C

data_7118029
_publ_section_title
;
 Paddlewheel 1,2,4-diazaphospholide dibismuthanes with very short
 bismuth-bismuth single bonds
;
_journal_name_full               Chem.Commun.
_journal_page_first              16184
_journal_paper_doi               10.1039/C5cc07064C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C32 H56 Bi2 N8 P4'
_chemical_formula_weight         1094.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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           SHELXL-97
_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.269(2)
_cell_angle_beta                 101.428(2)
_cell_angle_gamma                93.926(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5121(2)
_cell_length_b                   13.7719(3)
_cell_length_c                   15.2443(3)
_cell_measurement_reflns_used    7047
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.3440
_cell_measurement_theta_min      3.2420
_cell_volume                     2157.74(8)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26642
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  7.6550
_diffrn_standards_number         28968
_exptl_absorpt_coefficient_mu    8.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48) 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.457
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8798
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+1.1918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                6503
_reflns_number_total             8798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc07064c2.cif
_cod_data_source_block           150209-1
_cod_original_cell_volume        2157.73(8)
_cod_database_code               7118029