Methanol{tris[2-(2-pyridylmethyleneamino)ethyl]amino-κ^7^<i>N</i>}calcium(II) bis(perchlorate) methanol solvate
He, Hong-Shan; Acta Crystallographica Section E 63 (2007) m521–m522; doi:10.1107/S1600536807001626

data_2212020
_publ_section_title
;Methanol{tris[2-(2-pyridylmethyleneamino)ethyl]amino-\k^7^<i>N</i>}calcium(II)
 bis(perchlorate) methanol solvate
;
_journal_coeditor_code           BI2110
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m521
_journal_page_last               m522
_journal_paper_doi               10.1107/S1600536807001626
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Ca (C24 H27 N7) (C H4 O)] (Cl O4)2 , C H4 O'
_chemical_formula_moiety         'C25 H31 Ca N7 O 2+ , 2Cl O4 - , C H4 O'
_chemical_formula_sum            'C26 H35 Ca Cl2 N7 O10'
_chemical_formula_weight         716.59
_chemical_name_systematic
;
Methanol{tris[2-(2-pyridylmethyleneamino)ethyl]amino-\k^7^N}calcium(II)
bis(perchlorate) methanol solvate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3264(5)
_cell_length_b                   16.3163(4)
_cell_length_c                   10.9066(2)
_cell_measurement_reflns_used    7131
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     3261.28(13)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics
'WinGX and ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7131
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.644
_refine_ls_abs_structure_details 'Flack (1983), with 2509 Friedel pairs'
_refine_ls_abs_structure_Flack   0.58(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5546
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0963P)^2^+3.5065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                5077
_reflns_number_total             5546
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2110.cif
_cod_data_source_block           I
_cod_database_code               2212020
_cod_database_fobs_code          2212020