Crystal Growth of New Hexahydroxometallates Using a Hydroflux
W. Michael Chance; Daniel E. Bugaris; Athena S. Sefat; Hans-Conrad zur Loye; Inorganic Chemistry 52 (2013) 11723–11733; doi:10.1021/ic400910g

data_4336402
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia,SC,29208
USA
;
_publ_contact_author_email       zurloye@mail.chem.sc.edu
_publ_contact_author_fax         1-803-777-8508
_publ_contact_author_name        'Hans-Conrad zur Loye'
_publ_contact_author_phone       1-803-777-6916
_publ_section_title
;
 Crystal Growth of New Hexahydroxometallates Using a Hydroflux
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11723
_journal_page_last               11733
_journal_paper_doi               10.1021/ic400910g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Cu H6 O6, 2(Ba)'
_chemical_formula_sum            'Ba2 Cu H6 O6'
_chemical_formula_weight         440.27
_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   refall
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0341(12)
_cell_length_b                   6.4384(13)
_cell_length_c                   8.3844(17)
_cell_measurement_reflns_used    3539
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      31.96
_cell_measurement_theta_min      3.99
_cell_volume                     325.42(11)
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT+ version 6.22 (Bruker, 2001)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2012)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5246
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.08
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    15.167
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
'SADABS version 2008/1 (Sheldrick, 2008)' 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.493
_exptl_crystal_description       prism
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.537
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.0431(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1097
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+0.0811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0333
_reflns_number_gt                1036
_reflns_number_total             1097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400910g_si_002_6.cif
_cod_data_source_block           Ba2Cu(OH)6
_cod_database_code               4336402