Metal Complexes (M = Zn, Sn, and Pb) of 2-Phosphinobenzenethiolates: Insights into Ligand Folding and Hemilability
Brian M. Barry; Benjamin W. Stein; Christopher A. Larsen; Melissa N. Wirtz; William E. Geiger; Rory Waterman; Richard A. Kemp; Inorganic Chemistry 52 (2013) 9875–9884; doi:10.1021/ic400990n

data_4335827
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
MSC03 2060, 1 University of New Mexico
Albuquerque, NM 87131, USA
;
_publ_contact_author_email       rakemp@unm.edu
_publ_contact_author_name        'Richard A. Kemp'
_publ_contact_author_phone       505-272-7609
_publ_section_title
;
 Metal Complexes (M = Zn, Sn, and Pb) of 2-Phosphinobenzenethiolates:
 Insights into Ligand Folding and Hemilability
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9875
_journal_page_last               9884
_journal_paper_doi               10.1021/ic400990n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C28 H44 O2 P2 Sn'
_chemical_formula_weight         593.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.782(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6554(15)
_cell_length_b                   12.5442(10)
_cell_length_c                   14.4723(11)
_cell_measurement_reflns_used    4166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.13
_cell_measurement_theta_min      2.87
_cell_volume                     2933.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1332
_diffrn_reflns_av_sigmaI/netI    0.1121
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50227
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  0.8741
_exptl_absorpt_correction_T_min  0.7821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'bruker sadabs'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.123
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                3968
_reflns_number_total             7007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400990n_si_002_06.cif
_cod_data_source_block           Compound_8
_cod_database_code               4335827