Molybdenum(VI)cis-dioxo complexes bearing sugar derived chiral Schiff-base ligands: synthesis, characterization, and catalytic applications
Jin Zhao; Xiangge Zhou; Ana M. Santos; Eberhardt Herdtweck; Carlos C. Romão; Fritz E. Kühn; Dalton Trans.  (2003) 3736–3742; doi:10.1039/b306039j

data_7013267
_publ_section_title
;
 Molybdenum(VI)cis-dioxo complexes bearing sugar derived chiral
 Schiff-base ligands: synthesis, characterization, and catalytic
 applications
;
_journal_issue                   19
_journal_name_full               'Dalton Trans.'
_journal_page_first              3736
_journal_page_last               3742
_journal_paper_doi               10.1039/b306039j
_journal_year                    2003
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C21 H24 Cl N O10'
_chemical_formula_sum            'C21 H24 Cl N O10'
_chemical_formula_weight         485.86
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.2552(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2573(1)
_cell_length_b                   7.1473(1)
_cell_length_c                   14.4914(2)
_cell_measurement_reflns_used    2301
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      1.53
_cell_volume                     1166.40(3)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25017
_diffrn_reflns_theta_full        25.28
_diffrn_reflns_theta_max         25.28
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.89
_exptl_crystal_size_min          0.66
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0446P)^2^+0.2249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                4183
_reflns_number_total             4229
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b306039j.txt
_cod_data_source_block           ZHAG-4241-173
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7013267