Tetrakis(1,10-phenanthroline)calcium(II) bis(perchlorate) 4-(dimethylamino)benzaldehyde disolvate
Xi-Shi Tai; Jie Yin; Ming-Yang Hao; Acta Crystallographica Section E 63 (2007) m1827–m1827; doi:10.1107/S1600536807027055

data_2214219
_publ_section_title
;
 Tetrakis(1,10-phenanthroline)calcium(II) bis(perchlorate)
 4-(dimethylamino)benzaldehyde disolvate
;
_journal_coeditor_code           HB2432
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1827
_journal_page_last               m1827
_journal_paper_doi               10.1107/S1600536807027055
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ca (C12 H8 N2)4] (Cl O4)2, 2C9 H11 N O'
_chemical_formula_moiety         'C48 H32 Ca N8 2+, 2(Cl O4 -), 2(C9 H11 N O)'
_chemical_formula_sum            'C66 H54 Ca Cl2 N10 O10'
_chemical_formula_weight         1258.17
_chemical_name_systematic
;
Tetrakis(1,10-phenanthroline)calcium(II) bis(perchlorate)
4-(dimethylamino)benzaldehyde disolvate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            8
_cell_length_a                   17.455(3)
_cell_length_b                   17.455(3)
_cell_length_c                   38.952(3)
_cell_measurement_reflns_used    2661
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.49
_cell_measurement_theta_min      2.66
_cell_volume                     11868(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \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  0.1033
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            29937
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.562
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.2233
_refine_ls_R_factor_gt           0.0785
_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^)+(0.1079P)^2^+113.9196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.3877
_reflns_number_gt                1808
_reflns_number_total             5234
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2432.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2214219
_cod_database_fobs_code          2214219