(5-Carboxy-1<i>H</i>-pyrazole-3-carboxylato-κ^2^<i>N</i>^2^,<i>O</i>^3^)bis(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')cobalt(III) perchlorate 2.5-hydrate
Xie, Hui-Dong; Xie, Cheng-Zhi; Wang, Xiao-Qing; Shen, Guang-Qiu; Shen, De-Zhong; Acta Crystallographica Section E 63 (2007) m1477–m1479; doi:10.1107/S1600536807018703

data_2213203
_publ_section_title
;(5-Carboxy-1<i>H</i>-pyrazole-3-carboxylato-\k^2^<i>N</i>^2^,<i>O</i>^3^)bis(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')cobalt(III)
 perchlorate 2.5-hydrate
;
_journal_coeditor_code           CI2317
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1477
_journal_page_last               m1479
_journal_paper_doi               10.1107/S1600536807018703
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Co (C5 H2 N2 O4) (C12 H8 N2)2] Cl O4, 2.5H2 O'
_chemical_formula_moiety         'C29 H18 Co N6 O4 +, Cl O4 -, 2.5H2 O'
_chemical_formula_sum            'C29 H23 Cl Co N6 O10.5'
_chemical_formula_weight         717.91
_chemical_name_systematic
;
(5-Carboxy-1H-pyrazole-3-carboxylato-\k^2^N^2^,O^3^)bis(1,10-phenanthroline-
\k^2^N,N')cobalt(III) perchlorate 2.5-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.905(7)
_cell_length_b                   9.6566(19)
_cell_length_c                   23.237(5)
_cell_measurement_reflns_used    5351
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.11
_cell_volume                     5870(3)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_reduction        RAPID-AUTO
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP area-detector'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27567
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.8661
_exptl_absorpt_correction_T_min  0.8022
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.514
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6717
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0727P)^2^+6.0669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                5351
_reflns_number_total             6717
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2317.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_cell_volume        5870(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2213203
_cod_database_fobs_code          2213203