Synthetic, Structural, NMR, and Computational Study of a Geminally Bis(peri-substituted) Tridentate Phosphine and Its Chalcogenides and Transition-Metal Complexes
Matthew J. Ray; Rebecca A. M. Randall; Kasun S. Athukorala Arachchige; Alexandra M. Z. Slawin; Michael Bühl; Tomas Lebl; Petr Kilian; Inorganic Chemistry 52 (2013) 4346–4359; doi:10.1021/ic3024875

data_4334450
_publ_section_title
;
 Synthetic, Structural, NMR, and Computational Study of a Geminally
 Bis(peri-substituted) Tridentate Phosphine and Its Chalcogenides and
 Transition-Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4346
_journal_page_last               4359
_journal_paper_doi               10.1021/ic3024875
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C42 H57 O P3 S3'
_chemical_formula_sum            'C42 H57 O P3 S3'
_chemical_formula_weight         767.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-08-24
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.872(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.969(5)
_cell_length_b                   13.057(3)
_cell_length_c                   20.051(6)
_cell_measurement_reflns_used    13590
_cell_measurement_temperature    125
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.91
_cell_volume                     4123(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 28.944
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1358
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30858
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1640.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.930
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7255
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1313
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1171P)^2^+14.8236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3311
_reflns_number_gt                5583
_reflns_number_total             7257
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic3024875_si_001_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        4122.7(19)
_cod_database_code               4334450