A <i>cis</i>-Dioxomolybdenum(VI) Complex, [Mo{N~2~C~3~H~3~C(Me)~2~O}~2~(O)~2~]
Ehlert, Martin K.; Rettig, Steven J.; Storr, Alan; Trotter, James; Acta Crystallographica Section C 54 (1998) 473–475; doi:10.1107/S0108270197015898

data_2007167
_publ_section_title
;
 A <i>cis</i>-Dioxomolybdenum(VI) Complex,
 [Mo{N~2~C~3~H~3~C(Me)~2~O}~2~(O)~2~]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              473
_journal_page_last               475
_journal_paper_doi               10.1107/S0108270197015898
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Mo(O)2 (C6 H9 N2 O1)2]'
_chemical_formula_moiety         'C12 H18 Mo N4 O4 '
_chemical_formula_sum            'C12 H18 Mo N4 O4'
_chemical_formula_weight         378.24
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_cell_angle_alpha                90
_cell_angle_beta                 100.801(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.381(3)
_cell_length_b                   7.697(3)
_cell_length_c                   14.2869(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      17.7
_cell_volume                     1553.4(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1989)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1995)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'direct methods via SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Rigaku AFC-6S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3105
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         32.53
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        6.2
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Matthews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         '2.6 e \%A^-3^ (0.56\%A from Mo)'
_refine_diff_density_min         '-5.3 e \%A^-3^ (at Mo site)'
_refine_ls_abs_structure_details
;
refinement of the other polarity gave slightly higher R factors
(R = 0.0278 and wR = 0.0556)
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2811
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.027
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(F~o~)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.053
_reflns_number_gt                1766
_reflns_number_total             2811
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fg1386.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F~o~)^2^]' 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^(F~o~)^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1553.4(5)
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C12 H18 Mo N4 O4 '
_cod_database_code               2007167