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_4312248
_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 Ba O4 P2 Si4'
_chemical_formula_weight         904.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.935(2)
_cell_angle_beta                 100.147(2)
_cell_angle_gamma                111.752(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4765(6)
_cell_length_b                   11.7093(8)
_cell_length_c                   12.9960(8)
_cell_measurement_reflns_used    8684
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.237
_cell_measurement_theta_min      2.375
_cell_volume                     1203.59(14)
_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 0.982
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'fine-slice \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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10075
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                4800
_reflns_number_total             5316
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048978asi20040728_063537_4.cif
_cod_data_source_block           8
_cod_original_cell_volume        1203.59(13)
_cod_database_code               4312248