Dinuclear Calcium Complex with Weakly NH...O Hydrogen-Bonded Sulfonate Ligands
Akira Onoda; Yusuke Yamada; Mototsugu Doi; Taka-aki Okamura; Norikazu Ueyama; Inorganic Chemistry 40 (2001) 516–521; doi:10.1021/ic0003067

data_4319192
_publ_section_title
;
 Dinuclear Calcium Complex with Weakly NH...O Hydrogen-Bonded Sulfonate
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              516
_journal_page_last               521
_journal_paper_doi               10.1021/ic0003067
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C22 H36 Ca N2 O12 S2'
_chemical_formula_weight         624.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.67(1)
_cell_angle_beta                 90.11(1)
_cell_angle_gamma                71.71(2)
_cell_formula_units_Z            2
_cell_length_a                   11.032(3)
_cell_length_b                   14.753(3)
_cell_length_c                   9.447(1)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      10.2
_cell_volume                     1449.0(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF92 (ORIENT)'
_diffrn_measured_fraction_theta_full 0.8791
_diffrn_measured_fraction_theta_max 0.8791
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.090
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4775
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_standards_decay_%        6.47
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.72
_refine_diff_density_min         -1.17
_refine_ls_extinction_coef       0.020(9)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   2.283
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     353
_refine_ls_number_reflns         3349
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.0044
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00250|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                3349
_reflns_number_total             4481
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ic0003067_2.cif
_cod_data_source_block           '[Ca(PBSA)2(H2O)4](PBSA)'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C22 H36 Ca N2 O12 S2 '
_cod_database_code               4319192