Novel Copper(II) Induced Formation of a Porphyrinogen Derivative: X-ray Structural, Spectroscopic, and Electrochemical Studies of Porphyrinogen Complexes of Cu(II) and Co(III) Complex of a Trispyrazolyl Tripodal Ligand
Sachindranath Paul; Anil Kumar Barik; Shie Ming Peng; Susanta Kumar Kar; Inorganic Chemistry 41 (2002) 5803–5809; doi:10.1021/ic0112185

data_4318748
_publ_section_title
;
 Novel Copper(II) Induced Formation of a Porphyrinogen Derivative: X-ray
 Structural, Spectroscopic, and Electrochemical Studies of Porphyrinogen
 Complexes of Cu(II) and Co(III) Complex of a Trispyrazolyl Tripodal
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5803
_journal_page_last               5809
_journal_paper_doi               10.1021/ic0112185
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C20 H26 Cu N10 O11'
_chemical_formula_weight         646.05
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.58(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.476(3)
_cell_length_b                   9.4116(8)
_cell_length_c                   14.204(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.00
_cell_measurement_theta_min      8.80
_cell_volume                     2482.0(7)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w--2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2194
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 3
_diffrn_standards_interval_time  60
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.6731
_exptl_absorpt_correction_T_min  0.6252
_exptl_absorpt_correction_type   'empirical used psi-scan'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0653P)^2^+2.0819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                1571
_reflns_number_total             2194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112185_2.cif
_cod_data_source_block           ic7699
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4318748