Metal distribution and disorder in the crystal structure of [NH~2~Et~2~][Cr~7~<i>M</i>F~8~(^<i>t^</i>BuCO~2~)~16~] wheel molecules for <i>M</i> = Mn, Fe, Co, Ni, Cu, Zn and Cd
Larsen, Finn Krebs; Overgaard, Jacob; Christensen, Mogens; McIntyre, Garry James; Timco, Grigore; Winpenny, Richard E. P.; Acta Crystallographica Section B 70 (2014) 932–941; doi:10.1107/S2052520614019179

data_2105996
_publ_section_title
;
 Metal distribution and disorder in the crystal structure of
 [NH~2~Et~2~][Cr~7~<i>M</i>F~8~(^<i>t^</i>BuCO~2~)~16~] wheel molecules
 for <i>M</i> = Mn, Fe, Co, Ni, Cu, Zn and Cd
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              932
_journal_page_last               941
_journal_paper_doi               10.1107/S2052520614019179
_journal_volume                  70
_journal_year                    2014
_chemical_formula_sum            'C85.39 H157.49 Cd0.89 Cr7.11 F8 N O33.5'
_chemical_formula_weight         2364.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 111.2230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.0715(6)
_cell_length_b                   16.5459(4)
_cell_length_c                   31.1595(8)
_cell_measurement_temperature    273(2)
_cell_volume                     12049.3(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            225916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.516
_exptl_absorpt_coefficient_mu    0.849
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_F_000             4921
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.390
_refine_diff_density_min         -0.988
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         24551
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+99.2283P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.2101
_reflns_number_gt                18497
_reflns_number_total             24551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pi5020sup1.cif
_cod_data_source_block           cr7cd_doubleMmodel_slut
_cod_original_formula_sum        'C85.39 H157.49 Cd0.89 Cr7.11 F8 N O33.50'
_cod_database_code               2105996
_cod_database_fobs_code          2105996
_shelx_res_checksum              80548
_shelxl_version_number           20.13