Ni(ii) N4-macrocycle grafted crown ether: caesium cobalt(iii) bis(dicarbollide) coordination polymer
Malic, Nino; Nichols, Peter J.; Raston, Colin L.; Chemical Communications  (2002) 16–; doi:10.1039/b108162d

data_7114552
_publ_section_title
;
 Ni(ii) N4-macrocycle grafted crown ether: caesium cobalt(iii)
 bis(dicarbollide) coordination polymer
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              16
_journal_paper_doi               10.1039/b108162d
_journal_year                    2002
_chemical_formula_sum            'C48 H76 B18 Cl2 Co Cs N4 Ni O9'
_chemical_formula_weight         1369.16
_chemical_name_common
;
{cesium (cyclic hexaethylether Ni(TMTAA) diester)}{cobalt(III) 
bis(dicarbollide}{dichloromethane}{toluene}
;
_chemical_name_systematic
; 
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.067(2)
_cell_length_b                   17.667(4)
_cell_length_c                   29.266(6)
_cell_measurement_temperature    123(2)
_cell_volume                     6239(2)
_computing_cell_refinement       DENZO
_computing_data_collection       'Collect (Enraf-Nonius)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    X-Seed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'Phi and Omega scan'
_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  0.0979
_diffrn_reflns_av_sigmaI/netI    0.1265
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            57742
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.8309
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.267
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         14823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.826
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+2.3290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                9735
_reflns_number_total             14823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108162d.txt
_cod_data_source_block           c:\
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7114552