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_4348853
_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         'C44.73 H76.7 N12 O2 W2, 3.3(H)'
_chemical_formula_sum            'C46 H80 N12 O2 W2'
_chemical_formula_weight         1200.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.688(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.773(4)
_cell_length_b                   18.025(8)
_cell_length_c                   14.571(6)
_cell_measurement_reflns_used    6520
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.39
_cell_volume                     2537.4(19)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SMART (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15274
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.578
_exptl_absorpt_correction_T_max  0.5467
_exptl_absorpt_correction_T_min  0.4612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2004'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.674
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0394P)^2^+2.7991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                4000
_reflns_number_total             4911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01728_si_001.cif
_cod_data_source_block           W2_CO_2_TMhpp2_TMhpp2
_cod_original_cell_volume        2537.2(19)
_cod_database_code               4348853
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.044) H2B(0.044) H4A(0.064) H4B(0.064) H5A(0.066) H5B(0.066)
 H7A(0.044) H7B(0.044) H8A(0.08) H8B(0.08) H8C(0.08) H9A(0.103) H9B(0.103)
 H9C(0.103) H10A(0.1) H10B(0.1) H10C(0.1) H11A(0.111) H11B(0.111) H11C(0.111)
 H13A(0.048) H13B(0.048) H15A(0.07) H15B(0.07) H16A(0.081) H16B(0.081)
 H19A(0.095) H19B(0.095) H19C(0.095) H20A(0.102) H20B(0.102) H20C(0.102)
 H21A(0.133) H21B(0.133) H21C(0.133) H15C(0.07) H15D(0.07) H16C(0.081)
 H16D(0.081) H19D(0.095) H19E(0.095) H19F(0.095) H20D(0.102) H20E(0.102)
 H20F(0.102) H21D(0.133) H21E(0.133) H21F(0.133) H18A(0.057) H18B(0.057)
 H22A(0.152) H22B(0.152) H22C(0.152)
 Fixed X: H2A(0.7977) H2B(0.7871) H4A(0.5546) H4B(0.4552) H5A(0.4871)
 H5B(0.5431) H7A(0.7924) H7B(0.6573) H8A(0.5833) H8B(0.4518) H8C(0.5898)
 H9A(0.577) H9B(0.5882) H9C(0.449) H10A(0.8296) H10B(0.8432) H10C(0.7373)
 H11A(0.545) H11B(0.6479) H11C(0.5131) H13A(1.2249) H13B(1.0788) H15A(1.0664)
 H15B(0.971) H16A(0.812) H16B(0.9314) H19A(1.2778) H19B(1.3795) H19C(1.3049)
 H20A(1.2264) H20B(1.299) H20C(1.141) H21A(1.0542) H21B(1.0335) H21C(1.1099)
 H15C(1.2147) H15D(1.1394) H16C(0.9974) H16D(1.0866) H19D(1.0632) H19E(1.0876)
 H19F(0.9722) H20D(1.3787) H20E(1.3015) H20F(1.2804) H21D(0.8328) H21E(0.7008)
 H21F(0.7607) H18A(0.7681) H18B(0.8928) H22A(0.6958) H22B(0.8071) H22C(0.8121)
 Fixed Y: H2A(0.8299) H2B(0.7966) H4A(0.8035) H4B(0.8681) H5A(0.952)
 H5B(0.8763) H7A(1.0557) H7B(1.0567) H8A(0.8962) H8B(0.9065) H8C(0.9506)
 H9A(0.762) H9B(0.7269) H9C(0.7657) H10A(0.8904) H10B(0.9436) H10C(0.8765)
 H11A(0.9616) H11B(1.0301) H11C(1.0313) H13A(0.7941) H13B(0.7552) H15A(0.6966)
 H15B(0.7026) H16A(0.7913) H16B(0.7787) H19A(0.8186) H19B(0.7606) H19C(0.741)
 H20A(0.6227) H20B(0.6573) H20C(0.6342) H21A(0.8812) H21B(0.9622) H21C(0.9009)
 H15C(0.7986) H15D(0.7235) H16C(0.797) H16D(0.8647) H19D(0.6344) H19E(0.6455)
 H19F(0.6922) H20D(0.7046) H20E(0.6654) H20F(0.6359) H21D(0.7755) H21E(0.8274)
 H21F(0.7894) H18A(0.9421) H18B(0.9897) H22A(0.8977) H22B(0.9556) H22C(0.8724)
 Fixed Z: H2A(0.0888) H2B(-0.0126) H4A(-0.1205) H4B(-0.0979) H5A(-0.2253) H5B(-
 0.2605) H7A(-0.2432) H7B(-0.1952) H8A(0.1345) H8B(0.0575) H8C(0.0499)
 H9A(0.112) H9B(0.0137) H9C(0.0312) H10A(-0.252) H10B(-0.3367) H10C(-0.3496)
 H11A(-0.4076) H11B(-0.3963) H11C(-0.348) H13A(0.0797) H13B(0.0546) H15A(0.291)
 H15B(0.1929) H16A(0.2926) H16B(0.3775) H19A(0.2639) H19B(0.2281) H19C(0.3142)
 H20A(0.2149) H20B(0.1347) H20C(0.1146) H21A(0.4699) H21B(0.4276) H21C(0.3762)
 H15C(0.3023) H15D(0.3227) H16C(0.3989) H16D(0.3714) H19D(0.2062) H19E(0.1021)
 H19F(0.1416) H20D(0.2158) H20E(0.1252) H20F(0.2246) H21D(0.2924) H21E(0.2855)
 H21F(0.3812) H18A(0.2456) H18B(0.297) H22A(0.3952) H22B(0.4417) H22C(0.4769)
;