Syntheses and Structural Characterization of the (OCnOPor) Capped Porphyrins: Co(OC2OPor).CH2Cl2, Co(OC2OPor)(NO)out.0.46CHCl3, Co(OC3OPor).CHCl3, and Co(OC3OPor)(MeIm).3C7H8
Paul G. Jene; James A. Ibers; Inorganic Chemistry 39 (2000) 5796–5802; doi:10.1021/ic0006753

data_4321669
_publ_section_title
;
 Syntheses and Structural Characterization of the (OCnOPor) Capped
 Porphyrins: Co(OC2OPor).CH2Cl2, Co(OC2OPor)(NO)out.0.46CHCl3,
 Co(OC3OPor).CHCl3, and Co(OC3OPor)(MeIm).3C7H8
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5796
_journal_page_last               5802
_journal_paper_doi               10.1021/ic0006753
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C66 H56 Co N6 O8'
_chemical_formula_sum            'C87 H80 Co N6 O8'
_chemical_formula_weight         1396.5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.437(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.490(1)
_cell_length_b                   22.324(2)
_cell_length_c                   17.257(1)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      56.649
_cell_measurement_theta_min      4.945
_cell_volume                     6346.9(8)
_computing_cell_refinement       'SMART version 5.054 (Bruker, 1998)'
_computing_data_collection       'SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus version 6.02a (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL 5.101 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL 5.101 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72970
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated block'
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.12
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.71
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.71
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.082
_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^)+(0.04Fo^2^)^2^] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.151
_refine_ls_wR_factor_ref         0.160
_reflns_number_gt                8482
_reflns_number_total             11800
_reflns_threshold_expression     'I > 2sigma(I)'
_cod_data_source_file            ic0006753_4.cif
_cod_data_source_block           cmpd4
_cod_original_cell_volume        6346.8(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4321669