Hydrogen-Bonding Cavities about Metal Ions: Synthesis, Structure, and Physical Properties for a Series of Monomeric M-OH Complexes Derived from Water
Cora E. MacBeth; Brian S. Hammes; Victor G. Young,; A. S. Borovik; Inorganic Chemistry 40 (2001) 4733–4741; doi:10.1021/ic010250w

data_4320195
_publ_section_title
;
 Hydrogen-Bonding Cavities about Metal Ions: Synthesis, Structure, and
 Physical Properties for a Series of Monomeric M-OH Complexes Derived from
 Water
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4733
_journal_page_last               4741
_journal_paper_doi               10.1021/ic010250w
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'Prof. A. Borovik - University of Kansas'
_chemical_formula_sum            'C74 H158 Fe2 K4 N22 O16'
_chemical_formula_weight         1880.32
_chemical_name_common            99367a
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.096(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.663(3)
_cell_length_b                   11.4858(11)
_cell_length_c                   30.708(3)
_cell_measurement_temperature    173(2)
_cell_volume                     10391.1(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            76532
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         0.69
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         18400
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_obs          0.0531
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+11.8562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1380
_refine_ls_wR_factor_obs         0.1287
_reflns_number_observed          16198
_reflns_number_total             18401
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010250w_1.cif
_cod_data_source_block           99367a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+11.8562P] 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^)+(0.0583P)^2^+11.8562P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10391.2(17)
_cod_database_code               4320195