Di-μ-oxo-bis[(histidinato-κ^3^<i>N</i>,<i>N</i>,<i>O</i>)oxomolybdenum(V)] trihydrate
Ping-Fan Wu; Dong-Sheng Li; Xiang-Gao Meng; Xiao-Lin Zhong; Jiang Chao; Yu-Lin Zhu; Yong-Ge Wei; Acta Crystallographica Section E 61 (2005) m1553–m1555; doi:10.1107/S1600536805021732

data_2206399
_publ_section_title
;
 Di-\m-oxo-bis[(histidinato-\k^3^<i>N</i>,<i>N</i>,<i>O</i>)oxomolybdenum(V)]
 trihydrate
;
_journal_coeditor_code           CV6543
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1553
_journal_page_last               m1555
_journal_paper_doi               10.1107/S1600536805021732
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Mo2 (C6 H8 N3 O2)2 O4] , 3H2 O'
_chemical_formula_moiety         'C12 H16 Mo2 N6 O8 , 3H2 O'
_chemical_formula_sum            'C12 H22 Mo2 N6 O11'
_chemical_formula_weight         618.24
_chemical_name_systematic
;
Di-\m-oxo-bis[(histidinato-\k^3^N,N,O)oxomolybdenum(V)] trihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 113.136(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9594(12)
_cell_length_b                   8.7222(9)
_cell_length_c                   11.5783(12)
_cell_measurement_reflns_used    5483
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      3.02
_cell_volume                     1017.76(19)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5964
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.7807
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.686
_refine_ls_abs_structure_details 'Flack (1983), with 1006 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3372
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0218P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0486
_reflns_number_gt                3343
_reflns_number_total             3372
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6543.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2206399
_cod_database_fobs_code          2206399