Revisiting the synthesis of [Mo6(η5-C5Me5)O18]−. X-Ray structural analysis, UV-visible, electrochemical and multinuclear NMR characterization
Proust, Anna; Thouvenot, René; Herson, Patrick; Journal of the Chemical Society, Dalton Transactions  (1999) 51–; doi:10.1039/a805832f

data_7702340
_publ_contact_author
;   A. Proust Universite Pierre et Marie Curie
    4 Place Jussieu   Case 42
       75252 Paris Cedex 05
                             
;
_publ_section_title
;
 Revisiting the synthesis of [Mo6(\h5-C5Me5)O18]&#x2212;. X-Ray structural
 analysis, UV-visible, electrochemical and multinuclear NMR
 characterization
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              51
_journal_paper_doi               10.1039/a805832f
_journal_year                    1999
_chemical_formula_moiety         ' C29 H57 Mo6 O19 N1 '
_chemical_formula_sum            'C29 H57 Mo6 N O19'
_chemical_formula_weight         1299.4
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_audit_creation_date             98-03-27
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.406(16)
_cell_length_b                   16.065(9)
_cell_length_c                   21.851(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14.26
_cell_measurement_theta_min      13.92
_cell_volume                     4355(6)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4301
_diffrn_reflns_theta_max         25.
_diffrn_reflns_theta_min         1.
_diffrn_standards_decay_%        26.90
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  'one hour'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.70
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            ' red orange '
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             2295.84
_exptl_crystal_size_max          1.
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.36
_refine_diff_density_min         -1.65
_refine_ls_extinction_coef       140.6
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   3.4048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         2794
_refine_ls_R_factor_obs          0.0541
_refine_ls_shift/esd_max         1.388300
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0599
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_observed          2794
_reflns_number_total             4272
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            805832f.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_cell_measurement_temperature' value 'ambient' was changed
to '295(2)' -- the room/ambient temperature average [293;298] in
Kelvins(K) was taken.

data item '_symmetry_cell_setting' value 'Orthorhombic ' was changed
to 'orthorhombic' 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 '_atom_sites_solution_primary' value 'Direct_Methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4355(9)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C29 H57 Mo6 O19 N1 '
_cod_database_code               7702340