Cationic and Neutral Cp*M(NO)(κ(2)-Ph2PCH2CH2PPh2) Complexes of Molybdenum and Tungsten: Lewis-Acid-Induced Intramolecular C-H Activation.
Handford, Rex C.; Wakeham, Russell J.; Patrick, Brian O.; Legzdins, Peter; Inorganic chemistry 56 (2017) 3612–3622; doi:10.1021/acs.inorgchem.7b00027

data_4345312
_publ_section_title
;
 Cationic and Neutral Cp*M(NO)(\k(2)-Ph2PCH2CH2PPh2) Complexes of
 Molybdenum and Tungsten: Lewis-Acid-Induced Intramolecular C-H
 Activation.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3612
_journal_page_last               3622
_journal_paper_doi               10.1021/acs.inorgchem.7b00027
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety
'C43 H44 N2 O P2 W, C4 H10 O, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C51 H57 F6 N3 O8 P2 S2 W'
_chemical_formula_weight         1263.90
_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
_audit_creation_date             2016-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                97.659(10)
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_cell_length_a                   12.703(4)
_cell_length_b                   14.858(5)
_cell_length_c                   15.506(5)
_cell_measurement_reflns_used    9223
_cell_measurement_temperature    90(2)
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_cell_measurement_theta_min      2.66
_cell_volume                     2671.9(15)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'XT (Sheldrick, 2015)'
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_diffrn_detector                 'Bruker APEX2 area detector'
_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 0.993
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69523
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.170
_diffrn_reflns_theta_min         1.412
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_T_max  0.827
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_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0744 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8958.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         15695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.5464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13836
_reflns_number_total             15695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00027_si_002.cif
_cod_data_source_block           pl509
_cod_depositor_comments
'Adding full bibliography for 4345311--4345314.cif.'
_cod_original_cell_volume        2671.8(16)
_cod_database_code               4345312
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.702
_olex2_refinement_description
;
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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C49(H49A,H49B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              25199
_shelx_hkl_checksum              23269
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'