Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 5. Experimental and Theoretical Study of the Rotation Conformational Preferences of Mo2Cl4(R-py)4 (R-py = Substituted Pyridine) Molecules
F. Albert Cotton; Evgeny V. Dikarev; Jiande Gu; Santiago Herrero; Barbara Modec; Journal of the American Chemical Society 121 (1999) 11758–11761; doi:10.1021/ja992445x

data_4116645
_publ_section_title
;
 Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 5. Experimental
 and Theoretical Study of the Rotation Conformational Preferences of
 Mo2Cl4(R-py)4 (R-py = Substituted Pyridine) Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11758
_journal_page_last               11761
_journal_paper_doi               10.1021/ja992445x
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_moiety
;
 Mo2 Cl4 (N C5 H4 (C (C H3)3))4, (C H3)2 C O
;
_chemical_formula_structural     '(D2)-Mo2Cl4(4-t-Bu-py)4, (CH3)2CO'
_chemical_formula_sum            'C39 H58 Cl4 Mo2 N4 O'
_chemical_formula_weight         932.57
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(4-tert-butylpyridine))-di-molybdenum (II),
 D2-isomer, acetone solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 103.282(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.092(1)
_cell_length_b                   10.2150(2)
_cell_length_c                   28.944(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     9522.4(8)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20495
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6137
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_obs          0.0401
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+52.7557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1103
_refine_ls_wR_factor_obs         0.1028
_reflns_number_observed          5619
_reflns_number_total             6137
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja992445x.cif
_cod_data_source_block           JA992445X-178
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+52.7557P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+52.7557P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9522.4(7)
_cod_database_code               4116645