Complexes of the Heavier Alkaline Earth Metals Ca, Sr, and Ba with O-Functionalized Phosphanide Ligands
Stuart Blair; Keith Izod; William Clegg; Ross W. Harrington; Inorganic Chemistry 43 (2004) 8526–8531; doi:10.1021/ic048978a

data_4312247
_publ_section_title
;
 Complexes of the Heavier Alkaline Earth Metals Ca, Sr, and Ba with
 O-Functionalized Phosphanide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8526
_journal_page_last               8531
_journal_paper_doi               10.1021/ic048978a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C38 H72 O4 P2 Si4 Sr'
_chemical_formula_weight         854.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 118.471(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2184(18)
_cell_length_b                   17.818(3)
_cell_length_c                   12.5916(18)
_cell_measurement_reflns_used    10303
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.16
_cell_volume                     2409.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1249
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  0.8269
_exptl_absorpt_correction_T_min  0.7786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.256(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         10214
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                7400
_reflns_number_total             10214
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048978asi20040728_063537_3.cif
_cod_data_source_block           7
_cod_original_cell_volume        2409.7(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4312247