Synthesis of Heavy Cyclodipnictadiphosphanes [ClE(μ-P-Ter)]2 [E = P, As, Sb, or Bi; Ter = 2,6-bis(2,4,6-trimethylphenyl)phenyl].
Hinz, Alexander; Schulz, Axel; Villinger, Alexander; Inorganic chemistry 55 (2016) 3692–3699; doi:10.1021/acs.inorgchem.6b00218

data_4347480
_publ_section_title
;
 Synthesis of Heavy Cyclodipnictadiphosphanes [ClE(\m-P-Ter)]2 [E = P, As,
 Sb, or Bi; Ter = 2,6-bis(2,4,6-trimethylphenyl)phenyl].
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3692
_journal_page_last               3699
_journal_paper_doi               10.1021/acs.inorgchem.6b00218
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C48 H50 As2 P2'
_chemical_formula_sum            'C48 H50 As2 P2'
_chemical_formula_weight         838.66
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 107.141(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   38.646(3)
_cell_length_c                   13.2535(10)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    173(2)
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_cell_measurement_theta_min      2.46
_cell_volume                     4248.4(6)
_computing_cell_refinement       'Bruker Apex V7.51A'
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_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
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_diffrn_reflns_av_R_equivalents  0.0585
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_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.255
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_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         12374
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+2.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00218_si_002.cif
_cod_data_source_block           ah271a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347480
_shelx_estimated_absorpt_t_min   0.689
_shelx_estimated_absorpt_t_max   0.811
_shelxl_version_number           2013-4
_shelx_res_checksum              25843
_shelx_hkl_checksum              24640