A Homologous Series of Alkaline Earth Phosphanides: Syntheses, Crystal Structures, and Unusual Dynamic Behavior of (THF)nM[P{CH(SiMe3)2}(C6H4-2-CH2NMe2)]2 (M = Mg, Ca, Sr, Ba)
Stuart Blair; Keith Izod; William Clegg; Inorganic Chemistry 41 (2002) 3886–3893; doi:10.1021/ic0201194

data_4318255
_publ_section_title
;
 A Homologous Series of Alkaline Earth Phosphanides: Syntheses, Crystal
 Structures, and Unusual Dynamic Behavior of
 (THF)nM[P{CH(SiMe3)2}(C6H4-2-CH2NMe2)]2 (M = Mg, Ca, Sr, Ba)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3886
_journal_page_last               3893
_journal_paper_doi               10.1021/ic0201194
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H62 Ca N2 P2 Si4'
_chemical_formula_weight         689.22
_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                 91.673(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5550(4)
_cell_length_b                   17.4560(7)
_cell_length_c                   24.5782(10)
_cell_measurement_reflns_used    23241
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.26
_cell_volume                     4097.7(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34198
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         9539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0456P)^2^+1.6548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                7638
_reflns_number_total             9539
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0201194_2.cif
_cod_data_source_block           2
_cod_database_code               4318255