Nitrato[<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetrakis(1<i>H</i>-benzimidazol-2-ylmethyl)ethane-1,2-diamine]calcium(II) nitrate methanol trisolvate
Huang, Bei; Pei, Yamei; Wang, Li; Acta Crystallographica Section E 64 (2008) m1621–; doi:10.1107/S1600536808037859

data_2220103
_publ_section_title
;Nitrato[<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetrakis(1<i>H</i>-benzimidazol-2-ylmethyl)ethane-1,2-diamine]calcium(II)
 nitrate methanol trisolvate
;
_journal_coeditor_code           CI2674
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1621
_journal_paper_doi               10.1107/S1600536808037859
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ca (N O3) (C34 H32 N10)] N O3, 3C H4 O'
_chemical_formula_moiety         'C34 H32 Ca N11 O3 +, N O3 -, 3(C H4 O)'
_chemical_formula_sum            'C37 H44 Ca N12 O9'
_chemical_formula_weight         840.92
_chemical_name_systematic
;Nitrato[<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetrakis(1<i>H</i>-benzimidazol-
1-ylmethyl)ethane-1,2-diamine]calcium(II)
 nitrate methanol trisolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.5990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5945(4)
_cell_length_b                   25.3531(11)
_cell_length_c                   17.8402(7)
_cell_measurement_reflns_used    6962
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      2.20
_cell_volume                     4179.8(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.1461
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43547
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            pale-red
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.375
_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     575
_refine_ls_number_reflns         8189
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0978P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1705
_reflns_number_gt                4825
_reflns_number_total             8189
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2674.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2220103
_cod_database_fobs_code          2220103