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_4321255
_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            'C64 H64 Co N8 O4'
_chemical_formula_weight         1068.16
_chemical_name_common            Co(TpivPP)
_chemical_name_systematic
; 
 (\a,\a,\a,\a-tetrakis(o-pivalamidophenyl)
porphyrinato)cobalt(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 115.030(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.578(1)
_cell_length_b                   17.596(1)
_cell_length_c                   20.639(1)
_cell_measurement_reflns_used    7823
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.59
_cell_volume                     5784.2(5)
_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      153(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  0.039
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31330
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    'fixed with a riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         10754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.050
_refine_ls_shift/su_max          0.108
_refine_ls_shift/su_mean         0.004
_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          0.1156
_refine_ls_wR_factor_ref         0.122
_reflns_number_gt                7180
_reflns_number_total             10754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000127p_1.cif
_cod_data_source_block           cmpd1
_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_cell_volume        5784.3(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4321255