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_2105991
_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_coeditor_code           PI5020
_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 H157.5 Cr7.01 F8 Mn N O33.5'
_chemical_formula_weight         2307.09
_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                 110.356(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.9224(10)
_cell_length_b                   16.5198(7)
_cell_length_c                   30.8326(12)
_cell_measurement_temperature    273(2)
_cell_volume                     11901.4(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.514
_exptl_absorpt_coefficient_mu    0.796
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_F_000             4839
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.371
_exptl_crystal_size_min          0.242
_refine_diff_density_max         1.671
_refine_diff_density_min         -1.016
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1294
_refine_ls_number_reflns         21721
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+67.9675P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1952
_reflns_number_gt                16355
_reflns_number_total             21721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pi5020sup1.cif
_cod_data_source_block           cr7mn_single
_cod_original_formula_sum        'C85.39 H157.50 Cr7.01 F8 Mn N O33.50'
_cod_database_code               2105991
_cod_database_fobs_code          2105991
_shelx_res_checksum              2898
_shelxl_version_number           20.13