Exploring the Intricacies of Weak Interactions in Metal-Metal Bonds Using an Unsymmetrical Carbonyl Precursor and a Triple-Bonded W2(6+) Paddlewheel.
Chiarella, Gina M.; Feng, Chao; Murillo, Carlos A.; Zhao, Qinliang; Inorganic chemistry 55 (2016) 9471–9481; doi:10.1021/acs.inorgchem.6b01728

data_4348854
_publ_section_title
;
 Exploring the Intricacies of Weak Interactions in Metal-Metal Bonds Using
 an Unsymmetrical Carbonyl Precursor and a Triple-Bonded W2(6+)
 Paddlewheel.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9471
_journal_page_last               9481
_journal_paper_doi               10.1021/acs.inorgchem.6b01728
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C44 H80 N12 W2, 2(F6 P), 3(C H2 Cl2)'
_chemical_formula_sum            'C47 H86 Cl6 F12 N12 P2 W2'
_chemical_formula_weight         1689.62
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.097(3)
_cell_length_b                   19.113(3)
_cell_length_c                   34.639(6)
_cell_measurement_reflns_used    7689
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.29
_cell_volume                     13305(4)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SMART (Bruker, 2001)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1K 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  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            101370
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.820
_exptl_absorpt_correction_T_max  0.6571
_exptl_absorpt_correction_T_min  0.5154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2004'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.774
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.739
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         11781
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.745
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0330P)^2^+4.6895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                8655
_reflns_number_total             11781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01728_si_001.cif
_cod_data_source_block           W2_TMhpp4_PF6_4
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4348854