Cofacial Dicobalt Complex of a Binucleating Hexacarboxamide Cryptand Ligand
Glen E. Alliger; Peter Müller; Christopher C. Cummins; Daniel G. Nocera; Inorganic Chemistry 49 (2010) 3697–3699; doi:10.1021/ic100395a

data_4315352
_publ_section_title
;
 Cofacial Dicobalt Complex of a Binucleating Hexacarboxamide Cryptand
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3697
_journal_page_last               3699
_journal_paper_doi               10.1021/ic100395a
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C119 H176 Co2 K3 N9 O35.5'
_chemical_formula_weight         2535.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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-97
_cell_angle_alpha                93.1230(10)
_cell_angle_beta                 90.3350(10)
_cell_angle_gamma                115.4030(10)
_cell_formula_units_Z            2
_cell_length_a                   15.0760(3)
_cell_length_b                   17.0426(3)
_cell_length_c                   29.1340(5)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      2.88
_cell_volume                     6748.2(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            130252
_diffrn_reflns_theta_full        67.57
_diffrn_reflns_theta_max         67.57
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    3.384
_exptl_absorpt_correction_T_max  0.3447
_exptl_absorpt_correction_T_min  0.3113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
'Squeeze Reference: P. v.d. Sluis & A.L. Spek Acta Cryst. (1990), A46, 194.' 
'PLATON Reference: Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.'
'Complete FCF generated by Platon file given below.'
;
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2298
_refine_ls_number_reflns         23457
_refine_ls_number_restraints     10816
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1334P)^2^+3.7721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2178
_reflns_number_gt                18685
_reflns_number_total             23457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100395a_si_003_2.cif
_cod_data_source_block           d09067_pm_squeeze
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C119 H176 Co2 K3 N9 O35.50'
_cod_database_code               4315352
_cod_database_fobs_code          4315352