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_4312088
_publ_section_title
;
 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            'C23 H29 Cl3 Mo N4 O3'
_chemical_formula_weight         611.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   27.700(3)
_cell_length_b                   27.700(3)
_cell_length_c                   9.143(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.18
_cell_measurement_theta_min      5.23
_cell_volume                     6075.5(16)
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2766
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.38
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             2808
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.988
_refine_ls_goodness_of_fit_obs   0.990
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1777
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_restrained_S_obs      0.989
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_obs          0.0503
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+28.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1377
_refine_ls_wR_factor_obs         0.1266
_reflns_number_observed          1544
_reflns_number_total             1778
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic049130psi20040702_041847_1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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^)+(0.0900P)^2^+28.0000P] 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^)+(0.0900P)^2^+28.0000P] 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        6075.6(16)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4312088