Intramolecular Interactions Leading to Quasicubane Cages. Crystal Structure of [Mo2(NO)2(CO)4{μ-κ2;κ1-S2C(H)PCy3}2]
Daniel Miguel; Víctor Riera; Mei Wang; Claudette Bois; Sabine Halut; Inorganic Chemistry 37 (1998) 5944–5947; doi:10.1021/ic9713590

data_4323117
_publ_contact_author
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     DANIEL MIGUEL
     Departamento de Qu<i'>mica Inorg<a'>nica
     Facultad de Ciencias
     Universidad de Valladolid
     47005 VALLADOLID
     SPAIN
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_publ_contact_author_email       dmsj@sauron.quimica.uniovi.es
_publ_contact_author_fax         +34-83-423013
_publ_contact_author_phone       +34-83-423232
_publ_section_title
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 Intramolecular Interactions Leading to Quasicubane Cages. Crystal
 Structure of [Mo2(NO)2(CO)4{\m-\k2;\k1-S2C(H)PCy3}2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5944
_journal_page_last               5947
_journal_paper_doi               10.1021/ic9713590
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C42 H68 Mo2 S4 P2 O6 N2'
_chemical_formula_sum            'C42 H68 Mo2 N2 O6 P2 S4'
_chemical_formula_weight         1079.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             98-06-11
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 90.952
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.170(5)
_cell_length_b                   12.878(3)
_cell_length_c                   23.391(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      14
_cell_volume                     4870(2)
_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)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      294
_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  0.03
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9317
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        10.05
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.78
_exptl_crystal_colour            ' golden yellow '
_exptl_crystal_density_diffrn    1.47
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             2227.87
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.38
_refine_ls_extinction_coef       0.9(42)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.3076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         4033
_refine_ls_R_factor_obs          0.0368
_refine_ls_shift/esd_max         2.709425
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0399
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_observed          4033
_reflns_number_total             8558
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic9713590.cif
_cod_data_source_block           IC9713590
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        4870(4).
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C42 H68 Mo2 S4 P2 O6 N2 '
_cod_database_code               4323117