First structural characterization of a covalently bonded porphyrin‒carborane system
Vicente, M. Graça H.; Nurco, Daniel J.; Shetty, Shankar J.; Medforth, Craig J.; Smith, Kevin M.; Chemical Communications  (2001) 483–; doi:10.1039/b100231g

data_7114926
_publ_section_title
;
 First structural characterization of a covalently bonded
 porphyrin--carborane system
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              483
_journal_paper_doi               10.1039/b100231g
_journal_year                    2001
_chemical_formula_moiety         'C60 H84.8 B40 N4 Zn0.60, C6 H5 Cl'
_chemical_formula_sum            'C66 H89.8 B40 Cl N4 Zn0.6'
_chemical_formula_weight         1447.21
_chemical_name_common            'Zn(II) TMCP'
_chemical_name_systematic
; 
Zn(II) meso-Tetra[4-(1-methyl-o-carboranyl)methylphenyl]porphyrin 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.9630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3139(5)
_cell_length_b                   18.6428(8)
_cell_length_c                   15.7642(6)
_cell_measurement_reflns_used    5726
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.91
_cell_measurement_theta_min      2.18
_cell_volume                     3903.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33833
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count
;
Measured at the beginning and end of the data collection.
;
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.9223
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS 2.0 (Sheldrick, 2000) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pinacoid
_exptl_crystal_F_000             1486
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment
;
In the final model all hydrogen atom positions were treated with a riding 
model.  However, the freely refining position of H11 may be of interest.  
As such, the relevant geometrical distances involving riding and freely 
refining H11 are given below.

riding H11:
Zn1-H11, 2.09\%A
H11-B11, 1.12\%A

freely refining H11:
Zn1-H11, 2.16\%A
H11-B11, 1.06\%A
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8980
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+4.2585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1908
_reflns_number_gt                5896
_reflns_number_total             8980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100231g.txt
_cod_data_source_block           djn174s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C66 H89.8 B40 Cl N4 Zn0.60'
_cod_database_code               7114926