Synthesis and Characterization of a Series of Monometallo-, Bimetallo-, and Heterobimetallo-1,2-Ethene-Linked Cofacial Bisporphyrins
Todd E. Clement; Daniel J. Nurco; Kevin M. Smith; Inorganic Chemistry 37 (1998) 1150–1160; doi:10.1021/ic970774p

data_4322695
_publ_section_title
;
 Synthesis and Characterization of a Series of Monometallo-, Bimetallo-,
 and Heterobimetallo-1,2-Ethene-Linked Cofacial Bisporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1150
_journal_page_last               1160
_journal_paper_doi               10.1021/ic970774p
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C74 H88 N8 Cu Ni'
_chemical_formula_sum            'C74 H88 Cu N8 Ni'
_chemical_formula_weight         1211.77
_chemical_name_systematic
; 
cis-1-[Nickel (II) 5-(2,3,7,8,12,13,17,18-octaethylporphyrinyl)]-2-[Copper (II) 
5-(2,3,7,8,12,13,17,18-octaethylporphyrinyl)]ethene 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 108.64(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.169(3)
_cell_length_b                   13.875(2)
_cell_length_c                   22.660(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      5.22
_cell_volume                     6307(4)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens XCIF'
_computing_structure_refinement  'Siemens SHELXTL V. 5.03'
_computing_structure_solution    'Siemens SHELXTL V. 5.03'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Syntex P2~1~'
_diffrn_measurement_method       '\q - 2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9203
_diffrn_reflns_theta_max         57.08
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            'brick red'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.725
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_obs          0.0470
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+9.7021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1235
_refine_ls_wR_factor_obs         0.1201
_reflns_number_observed          7738
_reflns_number_total             8508
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970774p_1.cif
_cod_data_source_block           21xf
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+9.7021P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+9.7021P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6306.43(14)
_cod_original_formula_sum        'C74 H88 N8 Cu Ni'
_cod_database_code               4322695