Synthesis, spectroscopic studies and structural systematics of phosphine oxide complexes with Group II metal (beryllium?barium) nitrates
Davis, Martin F.; Levason, William; Ratnani, Raju; Reid, Gillian; Webster, Michael; New Journal of Chemistry 30 (2006) 782–; doi:10.1039/b600301j

data_7052251
_publ_section_title
;
 Synthesis, spectroscopic studies and structural systematics of
 phosphine oxide complexes with Group II metal (beryllium?barium)
 nitrates
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              782
_journal_paper_doi               10.1039/b600301j
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         'C60 H48 Ca N2 O10 P4'
_chemical_formula_structural     'Ca (N O3)2 (C30 H24 O2 P2)2'
_chemical_formula_sum            'C60 H48 Ca N2 O10 P4'
_chemical_formula_weight         1120.96
_chemical_name_systematic
;
Bis(nitrato-O,O')bis(1,2-bis(diphenylphosphinoyl)benzene)Calcium(II)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-11-01
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.394(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.771(4)
_cell_length_b                   10.6990(10)
_cell_length_c                   24.074(4)
_cell_measurement_reflns_used    52871
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     5431.5(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60223
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_correction_T_min  0.9322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         12261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                6807
_reflns_number_total             12261
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b600301j.txt
_cod_data_source_block           04rju008
_cod_original_cell_volume        5431.6(14)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7052251