Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 4. Rotational Isomers of Mo2Cl4(R-py)4 (R-py = 4-Picoline, 3,5-Lutidine, and 4-tert-Butylpyridine)
F. Albert Cotton; Evgeny V. Dikarev; Santiago Herrero; Barbara Modec; Inorganic Chemistry 38 (1999) 4882–4887; doi:10.1021/ic990728k

data_4322335
_publ_section_title
;
 Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 4. Rotational
 Isomers of Mo2Cl4(R-py)4 (R-py = 4-Picoline, 3,5-Lutidine, and
 4-tert-Butylpyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4882
_journal_page_last               4887
_journal_paper_doi               10.1021/ic990728k
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Mo2 Cl4 (N C5 H4 (C (C H3)3))4,C6 H6'
_chemical_formula_structural     (D2)-Mo2Cl4(4-t-Bu-py)4,C6H6
_chemical_formula_sum            'C42 H58 Cl4 Mo2 N4'
_chemical_formula_weight         952.60
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(4-tert-butylpyridine))-di-molybdenum (II),
 D2-isomer, benzene 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                 101.432(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.085(3)
_cell_length_b                   19.003(4)
_cell_length_c                   11.577(1)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.0
_cell_volume                     4546.6(12)
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9813
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.46
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.106
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2969
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.112
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_obs          0.0376
_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^)+(0.0299P)^2^+22.5464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0899
_refine_ls_wR_factor_obs         0.0843
_reflns_number_observed          2659
_reflns_number_total             2969
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990728k_1.cif
_cod_data_source_block           Mo2Cl4(4-t-Bu-py)4,C6H6_(3f,C6H6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+22.5464P] 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^)+(0.0299P)^2^+22.5464P] 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        4547(1)
_cod_database_code               4322335