Synthesis, properties and crystal structures of rigid porphyrins fused with bicyclo[2.2.2]octene units
Ito, Satoshi; Murashima, Takashi; Ono, Noboru; Uno, Hidemitsu; Chemical Communications  (1999) 2275–; doi:10.1039/a907460k

data_7110716
_publ_section_title
;
 Synthesis, properties and crystal structures of rigid porphyrins fused
 with bicyclo[2.2.2]octene units
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2275
_journal_paper_doi               10.1039/a907460k
_journal_year                    1999
_chemical_formula_analytical     'C69 H63 Cl3 N4 O1 Zn1 '
_chemical_formula_moiety         'C68 H60 N4 Zn, H2 O, C H Cl3 '
_chemical_formula_sum            'C69 H63 Cl3 N4 O Zn'
_chemical_formula_weight         1136.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.21(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.599(2)
_cell_length_b                   26.053(7)
_cell_length_c                   11.809(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.59
_cell_measurement_theta_min      11.14
_cell_volume                     2862.9(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution    DIRDIF94
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R '
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.09886
_diffrn_orient_matrix_UB_12      -0.00365
_diffrn_orient_matrix_UB_13      0.05195
_diffrn_orient_matrix_UB_21      0.04130
_diffrn_orient_matrix_UB_22      0.00095
_diffrn_orient_matrix_UB_23      -0.06991
_diffrn_orient_matrix_UB_31      0.00843
_diffrn_orient_matrix_UB_32      0.03820
_diffrn_orient_matrix_UB_33      0.00668
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.05262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7114
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0.49
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1188.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.947
_refine_ls_goodness_of_fit_ref   1.950
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0550
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                3158
_reflns_number_total             6734
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            907460ksup1.cif
_cod_data_source_block           '_2,2,2_porphyrin_zn_______'
_cod_depositor_comments
;
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_original_cell_volume        2863(1)
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_original_formula_sum        'C69 H63 Cl3 N4 O1 Zn1 '
_cod_database_code               7110716