Synthesis, Structures, and Solution Dynamics of Functionalized Phosphinomethanide Complexes of the Alkali Metals
Hill, M. N. Stuart; Izod, Keith; O'Shaughness, Paul; Clegg, William; Organometallics 19 (2000) 4531–; doi:10.1021/om000447g

data_4077556
_publ_section_title
;
 Synthesis, Structures, and Solution Dynamics of Functionalized
 Phosphinomethanide Complexes of the Alkali Metals
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4531
_journal_paper_doi               10.1021/om000447g
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C29 H52 N2 Na O1.5 P Si2'
_chemical_formula_weight         562.87
_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                 114.909(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0866(16)
_cell_length_b                   11.4896(11)
_cell_length_c                   18.9224(18)
_cell_measurement_reflns_used    8377
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.13
_cell_volume                     3369.3(6)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23890
_diffrn_reflns_theta_full        28.80
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         8133
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                4847
_reflns_number_total             8133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000447g.cif
_cod_data_source_block           ki32
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C29 H52 N2 Na O1.50 P Si2'
_cod_database_code               4077556