Oxidative stretching of metal-metal bonds to their limits.
Brogden, David W.; Turov, Yevgeniya; Nippe, Michael; Li Manni, Giovanni; Hillard, Elizabeth A.; Clérac, Rodolphe; Gagliardi, Laura; Berry, John F.; Inorganic chemistry 53 (2014) 4777–4790; doi:10.1021/ic5007204

data_4338166
_publ_section_title
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 Oxidative stretching of metal-metal bonds to their limits.
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_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4777
_journal_page_last               4790
_journal_paper_doi               10.1021/ic5007204
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'C40 H32 Mo N12 O W, C F3 O3 S, C4 H9 O, C2 H3 N, C24 H20 B'
_chemical_formula_sum            'C71 H64 B F3 Mo N13 O5 S W'
_chemical_formula_weight         1559.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                71.584(2)
_cell_angle_beta                 69.862(2)
_cell_angle_gamma                77.420(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0889(5)
_cell_length_b                   15.7173(5)
_cell_length_c                   16.9811(6)
_cell_measurement_temperature    100.0
_cell_volume                     3324.4(2)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
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_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56502
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.32
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  0.9215
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0600 before and 0.0359 after correction.
The Ratio of minimum to maximum transmission is 0.8436.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            '? brown'
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.088
_refine_diff_density_max         2.316
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         16600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+6.2505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                14695
_reflns_number_total             16600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5007204_si_001.cif
_cod_data_source_block           berry418_0m
_cod_depositor_comments
'Adding full bibliography for 4338161--4338168.cif.'
_cod_database_code               4338166
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Mo1, W1A}
{Mo1A, W1}
3. Uiso/Uaniso restraints and constraints
Uanis(Mo1) = Uanis(W1A)
Uanis(Mo1A) = Uanis(W1)
4. Others
 Sof(W1A)=Sof(Mo1A)=1-FVAR(1)
 Sof(W1)=Sof(Mo1)=FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=1-FVAR(2)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O3)=Sof(O4)=Sof(O5)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40),
  C42(H42), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61),
  C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
5.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C71(H71A,H71B,H71C)
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