Paddlewheel 1,2,4-diazaphospholide distibines with the shortest antimony-antimony single bonds.
Zhao, Minggang; Wang, Lixia; Zhang, Xiang; Zheng, Wenjun; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10505–10509; doi:10.1039/c6dt02039a

data_7039452
_publ_section_title
;
 Paddlewheel 1,2,4-diazaphospholide distibines with the shortest
 antimony-antimony single bonds.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10505
_journal_page_last               10509
_journal_paper_doi               10.1039/c6dt02039a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C63 H96 N8 P4 Sb2'
_chemical_formula_weight         1332.86
_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
;
2016-05-21 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                102.330(2)
_cell_angle_beta                 106.292(2)
_cell_angle_gamma                104.337(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9130(3)
_cell_length_b                   11.8061(3)
_cell_length_c                   16.0228(4)
_cell_measurement_reflns_used    12152
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.7110
_cell_measurement_theta_min      3.1950
_cell_volume                     1828.71(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42583
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 1.00
_diffrn_standards_interval_time  5.93
_diffrn_standards_number         48107
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6954
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0745P)^2^+1.3543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                5862
_reflns_number_total             6954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02039a2.cif
_cod_data_source_block           151203-2a
_cod_depositor_comments
'Adding full bibliography for 7039448--7039452.cif.'
_cod_original_cell_volume        1828.71(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7039452
_oxdiff_exptl_absorpt_empirical_full_min 0.779
_oxdiff_exptl_absorpt_empirical_full_max 1.459
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;