Oxo-deficient dioxylene complexes of Mo(vi) containing 3,6-di-tert-butylcatechol
Liu, Cai-Ming; Restorp, Per; Nordlander, Ebbe; Pierpont, Cortlandt G.; Chemical Communications  (2001) 2686–; doi:10.1039/b108220e

data_7125526
_publ_section_title
;
 Oxo-deficient dioxylene complexes of Mo(vi) containing
 3,6-di-tert-butylcatechol
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2686
_journal_paper_doi               10.1039/b108220e
_journal_year                    2001
_chemical_compound_source        toluene
_chemical_formula_sum            'C30 H46 Mo O6 S'
_chemical_formula_weight         630.67
_chemical_name_common            MoO(DMSO)(3,6-DBCat)2
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.2170(10)
_cell_angle_beta                 90.0720(10)
_cell_angle_gamma                93.1140(10)
_cell_formula_units_Z            4
_cell_length_a                   12.2701(5)
_cell_length_b                   16.7146(7)
_cell_length_c                   18.4327(6)
_cell_measurement_reflns_used    578
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      42.34
_cell_measurement_theta_min      10.11
_cell_volume                     3771.9(3)
_computing_data_collection       'SMART CCD'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'CCD detector'
_diffrn_measurement_method       'SMART CCD'
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17741
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rhombic needle'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_obs          0.0656
_refine_ls_shift/esd_max         0.111
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2190
_refine_ls_wR_factor_obs         0.1879
_reflns_number_observed          6159
_reflns_number_total             10391
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108220e.txt
_cod_data_source_block           MoO(DMSO)(3,6-DBCat)2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7125526