Geminally Substituted Tris(acenaphthyl) and Bis(acenaphthyl) Arsines, Stibines, and Bismuthine: A Structural and Nuclear Magnetic Resonance Investigation.
Chalmers, Brian A.; Meigh, Christina B. E.; Nejman, Phillip S.; Bühl, Michael; Lébl, Tomáš; Woollins, J. Derek; Slawin, Alexandra M. Z.; Kilian, Petr; Inorganic chemistry 55 (2016) 7117–7125; doi:10.1021/acs.inorgchem.6b01079

data_4348230
_publ_section_title
;
 Geminally Substituted Tris(acenaphthyl) and Bis(acenaphthyl) Arsines,
 Stibines, and Bismuthine: A Structural and Nuclear Magnetic Resonance
 Investigation.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7117
_journal_page_last               7125
_journal_paper_doi               10.1021/acs.inorgchem.6b01079
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C59.5 H69 P2 Sb'
_chemical_formula_sum            'C59.5 H69 P2 Sb'
_chemical_formula_weight         967.90
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-10
_audit_creation_method           'by CrystalStructure 4.1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.780(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.3925(19)
_cell_length_b                   24.118(3)
_cell_length_c                   16.793(2)
_cell_measurement_reflns_used    14910
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.90
_cell_volume                     4993.6(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45387
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.296
_diffrn_reflns_theta_min         1.855
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2028.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9053
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0329P)^2^+2.6491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                8526
_reflns_number_total             9053
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic6b01079_si_002.cif
_cod_data_source_block           6
_cod_database_code               4348230
_shelx_res_checksum              58807
_shelx_hkl_checksum              64306