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_4318256
_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 N2 O P2 Si4 Sr'
_chemical_formula_weight         808.86
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.593(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0498(9)
_cell_length_b                   13.0180(8)
_cell_length_c                   24.3664(14)
_cell_measurement_reflns_used    12710
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.40
_cell_volume                     4619.8(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.943
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19445
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5459
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0460P)^2^+5.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                4498
_reflns_number_total             5459
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0201194_3.cif
_cod_data_source_block           3
_cod_database_code               4318256