Heptametallic Bowl-Shaped Complexes Derived from Conjugated Schiff-Base Macrocycles: Synthesis, Characterization, and X-ray Crystal Structures
Gallant, Amanda J.; Chong, Jonathan H.; MacLachlan, Mark J.; Inorganic Chemistry 45 (2006) 5248–5250; doi:10.1021/ic060352s

data_4332430
_publ_section_title
;
 Heptametallic Bowl-Shaped Complexes Derived from Conjugated Schiff-Base
 Macrocycles:&#x00A0; Synthesis, Characterization, and X-ray Crystal
 Structures
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5248
_journal_page_last               5250
_journal_paper_doi               10.1021/ic060352s
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C168 H194 N12 O50 Zn14'
_chemical_formula_weight         4096.53
_chemical_name_systematic
;
 ?
;
_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                 113.343(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.342(5)
_cell_length_b                   38.204(5)
_cell_length_c                   20.526(5)
_cell_measurement_reflns_used    9650
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.4585
_cell_measurement_theta_min      2.255
_cell_volume                     19686(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            90372
_diffrn_reflns_theta_full        23.80
_diffrn_reflns_theta_max         23.80
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         15013
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          4.243
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                9145
_reflns_number_total             15013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060352ssup2.cif
_cod_data_source_block           mm025sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
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_cod_database_code               4332430