μ-Oxido-bis{[2,2-bis(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)acetato-κ^3^<i>N</i>^2^,<i>O</i>,<i>N</i>^2'^]chloridooxidomolybdenum(V)} monohydrate
Golobič, Amalija; Čeh, Boris; Acta Crystallographica Section E 66 (2010) m1648–m1649; doi:10.1107/S1600536810045393

data_2228320
_publ_section_title
;
 \m-Oxido-bis{[2,2-bis(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)acetato-\k^3^<i>N</i>^2^,<i>O</i>,<i>N</i>^2'^]chloridooxidomolybdenum(V)}
 monohydrate
;
_journal_coeditor_code           GK2307
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1648
_journal_page_last               m1649
_journal_paper_doi               10.1107/S1600536810045393
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mo2 (C12 H15 N4 O2)2 Cl2 O3], H2 O'
_chemical_formula_moiety         'C24 H30 Cl2 Mo2 N8 O7, H2 O'
_chemical_formula_sum            'C24 H32 Cl2 Mo2 N8 O8'
_chemical_formula_weight         823.36
_chemical_name_systematic
;
\m-Oxido-bis{[2,2-bis(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)acetato-\
\k^3^<i>N</i>^2^,<i>O</i>,<i>N</i>^2'^]chloridooxidomolybdenum(V)} monohydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.68690(10)
_cell_length_b                   20.6499(2)
_cell_length_c                   21.0082(2)
_cell_measurement_reflns_used    7980
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     6371.43(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'XTAL3.6 (Hall <i>et al.</i>, 1999)'
_computing_structure_refinement  'XTAL3.6 (Hall <i>et al.</i>, 1999)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .064
_diffrn_reflns_av_sigmaI/netI    .034
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91066
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         .969
_refine_diff_density_min         -1.504
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.416
_refine_ls_goodness_of_fit_ref   1.16
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .067
_refine_ls_R_factor_gt           .038
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
A REGINA (Wang et al., 1985) weighting scheme using the normal equation of
the second order was applied for
individual reflections so that w= A(0,0) + A(1,0)V(F) + A(0,1)V(S)
+ A(2,0)V(F)^2^ + A(0,2)V(S)^2^ + A(1,1)V(F)V(S), where V(F)=
F~obs~/F~obs~(max), F~obs~(max)=  496.47 and V(S)=(sin\q/\l)/ ((sin\q/\l)(max)),
(sin\q/\l)(max)=.6495.
The parameters were:
A(0,0)  =         110.7607, A(1,0)  =         .7072179
A(0,1)  =        -502.5041, A(2,0)  =        -.0004053
A(1,1)  =        -1.637116, A(0,2)  =         576.1985
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .039
_refine_ls_wR_factor_ref         .028
_reflns_number_gt                5534
_reflns_number_total             7300
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            gk2307.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-p 2ac 2ab'
_cod_database_code               2228320
_cod_database_fobs_code          2228320