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_4347481
_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 H52 As Cl N P'
_chemical_formula_sum            'C48 H52 As Cl N P'
_chemical_formula_weight         784.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.8540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9653(5)
_cell_length_b                   14.5149(5)
_cell_length_c                   17.7782(6)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.19
_cell_volume                     4117.7(2)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_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'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            87150
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         1.687
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         14875
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+1.3067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10616
_reflns_number_total             14875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00218_si_002.cif
_cod_data_source_block           ah271f_TerNHAsClPHTer
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347481
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.885
_shelxl_version_number           2013-4
_shelx_res_checksum              83248
_shelx_hkl_checksum              17498