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_7125525
_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_formula_sum            'C14 H20 Mo0.5 O2.5'
_chemical_formula_weight         276.27
_chemical_name_systematic
; 
[MoO(3,6-DBCat)2]4 
;
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_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            16
_cell_length_a                   22.5679(15)
_cell_length_b                   22.5679(15)
_cell_length_c                   13.0099(12)
_cell_measurement_temperature    293(2)
_cell_volume                     6626.1(9)
_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       '\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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45323
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   'Semi-empirical from psi-scans'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.127
_refine_ls_goodness_of_fit_all   1.261
_refine_ls_goodness_of_fit_obs   1.373
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.297
_refine_ls_restrained_S_obs      1.373
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_obs          0.0584
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+13.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2116
_refine_ls_wR_factor_obs         0.1878
_reflns_number_observed          2713
_reflns_number_total             3824
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108220e.txt
_cod_data_source_block           '[MoO(3,6-DBCat)2]4'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' 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 '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+13.3000P] 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^)+(0.0889P)^2^+13.3000P] 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      P4/nnc
_cod_original_formula_sum        'C14 H20 Mo0.50 O2.50'
_cod_database_code               7125525