Solid-State Coordination Chemistry of Metal Oxides: Hydrothermal Synthesis and Structural Characterization of o-Phenanthroline-Ligated Copper- and Zinc-Molybdenum Oxides
Pamela J. Hagrman; Jon Zubieta; Inorganic Chemistry 38 (1999) 4480–4485; doi:10.1021/ic990340p

data_4322272
_publ_section_title
;
 Solid-State Coordination Chemistry of Metal Oxides: Hydrothermal
 Synthesis and Structural Characterization of o-Phenanthroline-Ligated
 Copper- and Zinc-Molybdenum Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4480
_journal_page_last               4485
_journal_paper_doi               10.1021/ic990340p
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C24 H16 Cu Mo4 N4 O13'
_chemical_formula_weight         1015.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.99
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5218(3)
_cell_length_b                   12.1113(4)
_cell_length_c                   22.0125(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2777.88(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART-CCD'
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17326
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.587
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.429
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.609
_refine_diff_density_min         -2.445
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.958
_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_restrained_S_obs      1.127
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_obs          0.0622
_refine_ls_shift/esd_max         -0.150
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1617
_refine_ls_wR_factor_obs         0.1484
_reflns_number_observed          4121
_reflns_number_total             6565
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990340p_1.cif
_cod_data_source_block           MOXI-27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0887P)^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^)+(0.0887P)^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 
;
_cod_original_cell_volume        2777.89(15)
_cod_database_code               4322272