Compounds with Two Metal-Metal Multiple Bonds: New Ways of Making Doublets into Cyclic Quartets
F. Albert Cotton; Lee M. Daniels; Isabelle Guimet; Robert W. Henning; Glenn T. Jordan; Chun Lin; Carlos A. Murillo; Arthur J. Schultz; Journal of the American Chemical Society 120 (1998) 12531–12538; doi:10.1021/ja982425f

data_4116901
_publ_section_title
;
 Compounds with Two Metal-Metal Multiple Bonds: New Ways of Making
 Doublets into Cyclic Quartets
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12531
_journal_page_last               12538
_journal_paper_doi               10.1021/ja982425f
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C93 H99 Mo4 N12 O12'
_chemical_formula_weight         1960.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                87.49(2)
_cell_angle_beta                 84.48(2)
_cell_angle_gamma                89.16(2)
_cell_formula_units_Z            2
_cell_length_a                   14.555(2)
_cell_length_b                   17.001(4)
_cell_length_c                   17.179(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      17.93
_cell_measurement_theta_min      13.99
_cell_volume                     4226.9(15)
_computing_cell_refinement       'CAD4 V5'
_computing_data_collection       'CAD4 V5'
_computing_data_reduction        XCAD4
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'Omega two-theta 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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11458
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2010
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         10732
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_obs          0.0586
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1613
_refine_ls_wR_factor_obs         0.1400
_reflns_number_observed          7668
_reflns_number_total             10734
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982425f_1.cif
_cod_data_source_block           CMPD_1X
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.0700P)^2^+20.0000P] 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^)+(0.0700P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116901