Synthesis and Structural Characterization of Homoleptic 1,2,4-Diazaphospholide Alkaline Earth Metal Complexes
Liu, Dongling; Wang, Yongli; Pi, Chengfu; Zheng, Wenjun; Organometallics 33 (2014) 6013–; doi:10.1021/om500621s

data_4084512
_publ_section_title
;
 Synthesis and Structural Characterization of Homoleptic
 1,2,4-Diazaphospholide Alkaline Earth Metal Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6013
_journal_paper_doi               10.1021/om500621s
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C30 H54 Ca1.5 N6 P3'
_chemical_formula_weight         651.82
_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                 104.926(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.638(6)
_cell_length_b                   22.436(9)
_cell_length_c                   21.756(8)
_cell_measurement_reflns_used    908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.373
_cell_measurement_theta_min      2.628
_cell_volume                     7847(5)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega 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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35046
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.9291
_exptl_absorpt_correction_T_min  0.9125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         15319
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                6430
_reflns_number_total             15319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500621s_si_001.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 4084511--4084513.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C30 H54 Ca1.50 N6 P3'
_cod_database_code               4084512