Molecular structure of (5,10,15,20-tetrabutyl-2,3,7,8,12,13,17,18-octaethylporphyrinato)nickel(II)—correlation of nonplanarity with frontier orbital shifts †
Senge, Mathias O.; Renner, Mark W.; Kalisch, Werner W.; Fajer, Jack; Journal of the Chemical Society, Dalton Transactions  (2000) 381–; doi:10.1039/a905927j

data_7008885
_publ_section_title
;
 Molecular structure of
 (5,10,15,20-tetrabutyl-2,3,7,8,12,13,17,18-octaethylporphyrinato)nickel(II)---correlation
 of nonplanarity with frontier orbital shifts&#x200A;&#x2020;
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              381
_journal_paper_doi               10.1039/a905927j
_journal_year                    2000
_chemical_formula_moiety         'C52 H76 N4 Ni'
_chemical_formula_sum            'C52 H76 N4 Ni'
_chemical_formula_weight         815.88
_chemical_name_common            Ni(II)TnBuOEP
_chemical_name_systematic
; 
 (5,10,15,20-Tetra(n-butyl)-2,3,7,8,12,13,17,18-
 octaethylporphyrinato)nickel(II) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 119.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.581(11)
_cell_length_b                   7.566(2)
_cell_length_c                   25.967(12)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      24
_cell_volume                     4540(3)
_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      126(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.457
_diffrn_measured_fraction_theta_max 0.457
_diffrn_measurement_device_type  'Syntex P21'
_diffrn_measurement_method       2theta-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3431
_diffrn_reflns_theta_full        57.08
_diffrn_reflns_theta_max         57.08
_diffrn_reflns_theta_min         3.83
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.6153
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   'empirical, XABS2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       n/d
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+15.2512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                2780
_reflns_number_total             3058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a905927j.txt
_cod_data_source_block           ms404
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/d' 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^)+(0.0780P)^2^+15.2512P] 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^)+(0.0780P)^2^+15.2512P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7008885