Preparation and Characterization of Chiral Copper 12-Metallacrown-4 Complexes, Inorganic Analogues of Tetraphenylporphyrinatocopper(II)
Jason A. Halfen; Jeffrey J. Bodwin; Vincent L. Pecoraro; Inorganic Chemistry 37 (1998) 5416–5417; doi:10.1021/ic9807386

data_4323113
_publ_section_title
;
 Preparation and Characterization of Chiral Copper 12-Metallacrown-4
 Complexes, Inorganic Analogues of Tetraphenylporphyrinatocopper(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5416
_journal_page_last               5417
_journal_paper_doi               10.1021/ic9807386
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C85 H100 Cl Cu11 N16 O42'
_chemical_formula_weight         2752.20
_chemical_name_systematic
; 
Cu(OAc)2[12-MC Cu(II)N(S-b-pheha) -4]/
CuCl[12-MC Cu(II)N(S-b-pheha) -4](Cu(OAc)3)
;
_space_group_IT_number           1
_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
_cell_angle_alpha                88.7370(10)
_cell_angle_beta                 76.0010(10)
_cell_angle_gamma                71.1350(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5406(3)
_cell_length_b                   13.8416(3)
_cell_length_c                   16.6932(4)
_cell_measurement_temperature    158(2)
_cell_volume                     2655.56(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30681
_diffrn_reflns_theta_max         29.38
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.449
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.031
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1397
_refine_ls_number_reflns         23856
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_obs          0.0376
_refine_ls_shift/esd_max         -5.057
_refine_ls_shift/esd_mean        0.089
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+2.1531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0905
_refine_ls_wR_factor_obs         0.0849
_reflns_number_observed          21543
_reflns_number_total             23856
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9807386.cif
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+2.1531P] 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^)+(0.0296P)^2^+2.1531P] 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        2655.57(11)
_cod_database_code               4323113