Terphenyl complexes of molybdenum and tungsten with quadruple metal-metal bonds and bridging carboxylate ligands.
Carrasco, Mario; Mendoza, Irene; Faust, Michelle; López-Serrano, Joaquín; Peloso, Riccardo; Rodríguez, Amor; Alvarez, Eleuterio; Maya, Celia; Power, Philip P.; Carmona, Ernesto; Journal of the American Chemical Society 136 (2014) 9173–9180; doi:10.1021/ja503750a

data_4122007
_publ_section_title
;
 Terphenyl complexes of molybdenum and tungsten with quadruple metal-metal
 bonds and bridging carboxylate ligands.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9173
_journal_page_last               9180
_journal_paper_doi               10.1021/ja503750a
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         '2(C48 H42 F6 Mo2 O4), C4 H10 O'
_chemical_formula_sum            'C100 H94 F12 Mo4 O9'
_chemical_formula_weight         2051.51
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                81.079(2)
_cell_angle_beta                 89.802(2)
_cell_angle_gamma                87.103(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7561(6)
_cell_length_b                   12.1811(6)
_cell_length_c                   33.4375(18)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.27
_cell_volume                     4322.4(4)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            105876
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.9375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.273
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         15456
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      2.319
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+13.6786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                11988
_reflns_number_total             15456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja503750a_si_001.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122003--4122009.cif.
;
_cod_database_code               4122007