Synchrotron X-ray study of [5,15-diphenyl-2,8,12,18-tetra-<i>n</i>-hexyl-3,7,13,17-tetramethylporphyrinato]nickel(II)
Bond, Andrew D.; Feeder, Neil; Redman, James E.; Teat, Simon J.; Sanders, Jeremy K. M.; Acta Crystallographica Section E 59 (2003) m818–m820; doi:10.1107/S1600536803018853

data_2203019
_publ_section_title
;Synchrotron X-ray study of
 [5,15-diphenyl-2,8,12,18-tetra-<i>n</i>-hexyl-3,7,13,17-tetramethylporphyrinato]nickel(II)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m818
_journal_page_last               m820
_journal_paper_doi               10.1107/S1600536803018853
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C60 H76 N4)]'
_chemical_formula_moiety         'C60 H76 N4 Ni'
_chemical_formula_sum            'C60 H76 N4 Ni'
_chemical_formula_weight         911.96
_chemical_name_systematic
;
[5,15-Diphenyl-2,8,12,18-tetra-n-hexyl-3,7,13,17-
tetramethylporphyrinato]nickel(II)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9640(10)
_cell_length_b                   18.4920(10)
_cell_length_c                   36.260(2)
_cell_measurement_reflns_used    35312
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      2.9
_cell_volume                     10027.3(10)
_computing_cell_refinement       'LSCELL (Clegg, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.90
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin-slice \w'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6891
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_sigmaI/netI    0.075
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            69934
_diffrn_reflns_theta_full        24.2
_diffrn_reflns_theta_max         29.5
_diffrn_reflns_theta_min         1.7
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.43
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Correction applied by SADABS (Sheldrick, 1997).
 Note that the transmission factors are not real since they
 include corrections for beam decay and possibly
 crystal decay (the two cannot be distinguished).
 The numbers listed in the CIF are those calculated by SHELXL.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.95
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         27810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.95
_refine_ls_R_factor_all          0.088
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0702P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.121
_refine_ls_wR_factor_ref         0.129
_reflns_number_gt                17657
_reflns_number_total             27810
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6170.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2203019
_cod_database_fobs_code          2203019