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_4318254
_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            'C36 H70 Mg N2 O P2 Si4'
_chemical_formula_weight         745.55
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.413(3)
_cell_length_b                   12.072(3)
_cell_length_c                   32.620(11)
_cell_measurement_reflns_used    22023
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.411
_cell_measurement_theta_min      2.465
_cell_volume                     4494(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART 1K 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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            38871
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         10677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.8386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                8590
_reflns_number_total             10677
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0201194_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        4495(2)
_cod_database_code               4318254