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_4322273
_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            'C12 H10 Cu Mo N2 O5'
_chemical_formula_weight         421.70
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.5860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0500(10)
_cell_length_b                   5.8818(4)
_cell_length_c                   16.2268(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1303.45(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7851
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.616
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.410
_refine_diff_density_min         -3.208
_refine_diff_density_rms         0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.2054
_reflns_number_gt                2135
_reflns_number_total             3063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990340p_2.cif
_cod_data_source_block           MOXI-28
_cod_database_code               4322273