Lithium Di- and Trimethyl Dimolybdenum(II) Complexes with Mo-Mo Quadruple Bonds and Bridging Methyl Groups.
Curado, Natalia; Carrasco, Mario; Álvarez, Eleuterio; Maya, Celia; Peloso, Riccardo; Rodríguez, Amor; López-Serrano, Joaquín; Carmona, Ernesto; Journal of the American Chemical Society 137 (2015) 12378–12387; doi:10.1021/jacs.5b07899

data_4124570
_publ_section_title
;
 Lithium Di- and Trimethyl Dimolybdenum(II) Complexes with Mo-Mo Quadruple
 Bonds and Bridging Methyl Groups.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12378
_journal_page_last               12387
_journal_paper_doi               10.1021/jacs.5b07899
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C53 H79 Mo2 N4, C16 H32 Li O4'
_chemical_formula_sum            'C69 H111 Li Mo2 N4 O4'
_chemical_formula_weight         1259.44
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.1710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.402(3)
_cell_length_b                   12.1781(9)
_cell_length_c                   27.374(2)
_cell_measurement_reflns_used    5381
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.42
_cell_measurement_theta_min      2.23
_cell_volume                     13808.4(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60299
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5376.0
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.564
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         13662
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+49.0653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                8666
_reflns_number_total             13662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b07899_si_002.cif
_cod_data_source_block           4c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        13808.5(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4124570