Changing cage structures through inter-ligand repulsions
Graham, Alasdair; Meier, Stephanie; Parsons, Simon; Winpenny, Richard E. P.; Chemical Communications  (2000) 811–; doi:10.1039/b000385i

data_7110848
_publ_section_title
;
 Changing cage structures through inter-ligand repulsions
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              811
_journal_paper_doi               10.1039/b000385i
_journal_year                    2000
_chemical_formula_moiety
; 
[Ni9(chp)3(Hchp)(OH)6(Me3NCH2CO2)9(CO3)Cl].[Ni(chp)3]4.0.5Cl.(chp.Hchp)1.5. 
8.5EtOAc 
;
_chemical_formula_sum            'C193.5 H240.5 Cl22.5 N30 Ni13 O65'
_chemical_formula_weight         5587.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   30.603(2)
_cell_length_b                   30.603(2)
_cell_length_c                   46.202(5)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     37473(5)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device
; 
Stoe Stadi-4 diffractometer with 
Oxford Cryosystems variable temperature device. 
;
_diffrn_measurement_method       Omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2318
_diffrn_reflns_av_sigmaI/netI    0.1599
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            10611
_diffrn_reflns_theta_max         56.00
_diffrn_reflns_theta_min         2.54
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.919
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       'plate developed in (001)'
_exptl_crystal_F_000             17268
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.886
_refine_ls_goodness_of_fit_obs   1.161
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         10466
_refine_ls_number_restraints     1025
_refine_ls_restrained_S_all      0.927
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_obs          0.0794
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2245
_refine_ls_wR_factor_obs         0.1824
_reflns_number_observed          4829
_reflns_number_total             10473
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000385isup1.cif
_cod_data_source_block           winsom
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1049P)^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^)+(0.1049P)^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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        37473.1(53)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C193.50 H240.50 Cl22.50 N30 Ni13 O65'
_cod_database_code               7110848