Mononuclear Ca(II)-Bulky Aryl-Phosphate Monoanion and Dianion Complexes with Ortho-Amide Groups
Akira Onoda; Yusuke Yamada; Taka-aki Okamura; Hitoshi Yamamoto; Norikazu Ueyama; Inorganic Chemistry 41 (2002) 6038–6047; doi:10.1021/ic010570f

data_4318805
_publ_section_title
;
 Mononuclear Ca(II)-Bulky Aryl-Phosphate Monoanion and Dianion Complexes
 with Ortho-Amide Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6038
_journal_page_last               6047
_journal_paper_doi               10.1021/ic010570f
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C166 H170 Ca N19 O25 P3'
_chemical_formula_weight         2964.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   19.128(4)
_cell_length_b                   19.128(4)
_cell_length_c                   27.937(7)
_cell_measurement_temperature    296
_cell_volume                     8852(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14441
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.129
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3128
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         13562
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.524
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.2490
_reflns_number_gt                5540
_reflns_number_total             13562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010570f_3.cif
_cod_data_source_block           3
_cod_database_code               4318805