Characterization and Crystal Structure of a Chiral Ruffled Basket-Handle Porphyrin
Philippe Richard; Eric Rose; Bernard Boitrel; Inorganic Chemistry 37 (1998) 6532–6534; doi:10.1021/ic980499m

data_4323199
_publ_section_title
;
 Characterization and Crystal Structure of a Chiral Ruffled Basket-Handle
 Porphyrin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6532
_journal_page_last               6534
_journal_paper_doi               10.1021/ic980499m
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C71 H77 N13 Ni O16'
_chemical_formula_weight         1427.17
_chemical_name_common            ArpyNi
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.933(2)
_cell_length_b                   17.598(3)
_cell_length_c                   16.996(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.03
_cell_measurement_theta_min      10.58
_cell_volume                     3685.3(11)
_computing_cell_refinement       CAD4-EXPRESS
_computing_data_collection       CAD4-EXPRESS
_computing_data_reduction        'XCAD4 (Harms, 1996) '
_computing_molecular_graphics    'ORTEP-3 '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8713
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         8428
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_obs          0.0575
_refine_ls_shift/esd_max         0.050
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1708
_refine_ls_wR_factor_obs         0.1567
_reflns_number_observed          7126
_reflns_number_total             8428
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980499m.cif
_cod_data_source_block           ArpyNi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+0.0000P] 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^)+(0.1310P)^2^+0.0000P] 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        3685.1(11)
_cod_database_code               4323199