Non-planar porphyrins with mixed substituent pattern: bromination and formylation of ethyl-substituted tetraphenylporphyrins and tetraalkylporphyrins
Senge, Mathias O.; Gerstung, Vanessa; Ruhlandt-Senge, Karin; Runge, Steffen; Lehmann, Ingo; Journal of the Chemical Society, Dalton Transactions  (1998) 4187–; doi:10.1039/a806460a

data_7027060
_publ_section_title
;
 Non-planar porphyrins with mixed substituent pattern: bromination and
 formylation of ethyl-substituted tetraphenylporphyrins and
 tetraalkylporphyrins
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4187
_journal_paper_doi               10.1039/a806460a
_journal_year                    1998
_chemical_formula_moiety
; 
 C53 H44 N4 Ni1 O1.0.75(C1 H1 Cl3).0.25(H2 O1)
;
_chemical_formula_sum            'C53.75 H45.25 Cl2.25 N4 Ni O1.25'
_chemical_formula_weight         905.66
_chemical_name_systematic
; 
 (2,3,12,13-Tetraethyl-7-formyl-5,10,15,20- 
 tetraphenylporphyrinato)nickel(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.401(17)
_cell_angle_beta                 73.099(16)
_cell_angle_gamma                69.047(17)
_cell_formula_units_Z            2
_cell_length_a                   12.579(3)
_cell_length_b                   13.882(3)
_cell_length_c                   14.383(3)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      55
_cell_measurement_theta_min      41
_cell_volume                     2241.8(9)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'XDISK, Shelxtl-Plus, Siemens 1994'
_computing_molecular_graphics    'XP, Shelxtl-Plus, Siemens 1994'
_computing_publication_material  'XCIF, Shelxtl-Plus, Siemens 1994'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2theta-theta
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6107
_diffrn_reflns_theta_full        56.45
_diffrn_reflns_theta_max         56.45
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.207
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.7331
_exptl_absorpt_correction_type   'empirical, XABS2'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       n/d
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5935
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1640
_refine_ls_R_factor_gt           0.1105
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1788P)^2^+11.6405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2818
_refine_ls_wR_factor_ref         0.3280
_reflns_number_gt                3725
_reflns_number_total             5935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            806460asup1.cif
_cod_data_source_block           ms408
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1788P)^2^+11.6405P] 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^)+(0.1788P)^2^+11.6405P] 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        2241.9(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027060