The Lengths of Molybdenum to Molybdenum Quadruple Bonds: Correlations, Explanations, and Corrections
F. Albert Cotton; Lee M. Daniels; Elizabeth A. Hillard; Carlos A. Murillo; Inorganic Chemistry 41 (2002) 2466–2470; doi:10.1021/ic025508c

data_4317975
_publ_section_title
;
 The Lengths of Molybdenum to Molybdenum Quadruple Bonds: Correlations,
 Explanations, and Corrections
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2466
_journal_page_last               2470
_journal_paper_doi               10.1021/ic025508c
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C32.50 H37 Cl Mo2 N8 O4'
_chemical_formula_structural     Mo2(C5H4NNC(O)CH2CH3)4,0.5CH2Cl2
_chemical_formula_sum            'C32.5 H37 Cl Mo2 N8 O4'
_chemical_formula_weight         831.03
_chemical_melting_point          ?
_chemical_name_systematic
;
tetrakis(N-pyridylpropionamide-N,N')dimolybdenum(II,II), dichloromethane 
solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.844(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.085(2)
_cell_length_b                   15.5627(13)
_cell_length_c                   21.863(2)
_cell_measurement_reflns_used    7492
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.525
_cell_measurement_theta_min      2.2875
_cell_volume                     6785.2(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL v5.05 (Siemens, 1996)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Bruker SMART area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35083
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.94925
_exptl_absorpt_correction_T_min  0.84330
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         11756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_obs          0.0314
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+2.8481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0809
_refine_ls_wR_factor_obs         0.0735
_reflns_number_observed          9465
_reflns_number_total             11924
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic025508c_s2_2.cif
_cod_data_source_block           compound2
_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 1569 2011-02-09 13:29:24Z 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^)+(0.0402P)^2^+2.8481P] 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^)+(0.0402P)^2^+2.8481P] 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        6785.4(10)
_cod_original_formula_sum        'C32.50 H37 Cl Mo2 N8 O4'
_cod_database_code               4317975