A Family of Dioxo-Molybdenum(VI) Complexes of N2X Heteroscorpionate Ligands of Relevance to Molybdoenzymes
Brian S. Hammes; Bal S. Chohan; Justin T. Hoffman; Simon Einwächter; Carl J. Carrano; Inorganic Chemistry 43 (2004) 7800–7806; doi:10.1021/ic049130p

data_4312090
_publ_section_title
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 A Family of Dioxo-Molybdenum(VI) Complexes of N2X Heteroscorpionate
 Ligands of Relevance to Molybdoenzymes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7800
_journal_page_last               7806
_journal_paper_doi               10.1021/ic049130p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C14 H21 Cl Mo N4 O2 S'
_chemical_formula_weight         440.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.397(3)
_cell_length_b                   15.147(4)
_cell_length_c                   8.658(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      5.11
_cell_volume                     1756.9(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1200
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.69
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             896
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0046(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1198
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_obs          0.0632
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+33.1445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_obs         0.1534
_reflns_number_observed          1130
_reflns_number_total             1200
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic049130psi20040702_041847_3.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+33.1445P] 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^)+(0.0309P)^2^+33.1445P] 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        1757.0(7)
_cod_database_code               4312090