Bis{tris[2-(2-oxidobenzylideneazaniumyl)ethyl]amine-κ^3^<i>O</i>,<i>O</i>',<i>O</i>''}calcium bis(perchlorate) acetonitrile disolvate
Kose, Muhammet; McKee, Vickie; Acta Crystallographica Section E 67 (2011) m149–; doi:10.1107/S1600536810053961

data_2229191
_publ_section_title
;
 Bis{tris[2-(2-oxidobenzylideneazaniumyl)ethyl]amine-\k^3^<i>O</i>,<i>O</i>',<i>O</i>''}calcium
 bis(perchlorate) acetonitrile disolvate
;
_journal_coeditor_code           PV2371
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m149
_journal_paper_doi               10.1107/S1600536810053961
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ca (C27 H30 N4 O3)2] (Cl O4)2 , 2C2 H3 N'
_chemical_formula_moiety
'C54 H60 Ca N8 O6 2+ , 2(C2 H3 N), 2(Cl O4 -)'
_chemical_formula_sum            'C58 H66 Ca Cl2 N10 O14'
_chemical_formula_weight         1238.19
_chemical_name_systematic
;
Bis{tris[2-(2-oxidobenzylideneazaniumyl)ethyl]amine-
\k^3^<i>O</i>,<i>O</i>',<i>O</i>''}calcium bis(perchlorate) acetonitrile
disolvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3469(7)
_cell_length_b                   19.5307(12)
_cell_length_c                   27.3178(16)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.21
_cell_volume                     6054.0(6)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55467
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+3.4246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                5810
_reflns_number_total             6915
_reflns_threshold_expression     'I > 2.0\s(I)'
_cod_data_source_file            pv2371.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               2229191
_cod_database_fobs_code          2229191