Structural Characterization of the Picket Fence (TpivPP) Porphyrins Co(TpivPP), Co(TpivPP)(NO2)(1-MeIm), and Co(TpivPP)(NO2)(1,2-Me2Im)
Paul G. Jene; James A. Ibers; Inorganic Chemistry 39 (2000) 3823–3827; doi:10.1021/ic000127p

data_4321256
_publ_section_title
;
 Structural Characterization of the Picket Fence (TpivPP) Porphyrins
 Co(TpivPP), Co(TpivPP)(NO2)(1-MeIm), and Co(TpivPP)(NO2)(1,2-Me2Im)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3823
_journal_page_last               3827
_journal_paper_doi               10.1021/ic000127p
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C68 H70 Co N11 O6'
_chemical_formula_weight         1196.28
_chemical_name_common            Co(TpivPP)(NO~2~)(1-MeIm)
_chemical_name_systematic
; 
 (nitro)(1-methylimidazolato)(\a,\a,\a,\a-tetrakis
(o-pivalamidophenyl)porphyrinato)cobalt(III)
;
_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
_cell_angle_beta                 90.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.522(4)
_cell_length_b                   18.942(4)
_cell_length_c                   18.177(4)
_cell_measurement_reflns_used    2859
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.54
_cell_volume                     6377(2)
_computing_cell_refinement       'SMART version 5.101 (Bruker, 1999)'
_computing_data_collection       'SMART version 5.101 (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus version 5.101 (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-99 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL-99 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-99 (Sheldrick, 1999)'
_computing_structure_solution    'SHELXS-99 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20074
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    'fixed with a riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
w = 1/[\s^2^(Fo^2^)+(0.04Fo^2^)^2^] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.120
_reflns_number_gt                2677
_reflns_number_total             5632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000127p_2.cif
_cod_data_source_block           cmpd2
_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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4321256