Controlled cis Labilization of CO from Manganese(I) Mixed Carbonyl/Isocyanide Complexes: An Entry Point to Coordinatively Unsaturated Metallo-Lewis Acids
Agnew, Douglas W.; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Organometallics 36 (2017) 363–; doi:10.1021/acs.organomet.6b00792

data_4086822
_publ_section_title
;
 Controlled cis Labilization of CO from Manganese(I) Mixed
 Carbonyl/Isocyanide Complexes: An Entry Point to Coordinatively
 Unsaturated Metallo-Lewis Acids
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              363
_journal_paper_doi               10.1021/acs.organomet.6b00792
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C66 H77 Mn N2 O4'
_chemical_formula_sum            'C66 H77 Mn N2 O4'
_chemical_formula_weight         1017.23
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.862(2)
_cell_length_b                   16.736(2)
_cell_length_c                   41.454(5)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.42
_cell_volume                     11520(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            87844
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.416
_diffrn_reflns_theta_max         24.416
_diffrn_reflns_theta_min         0.998
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.2582
_exptl_absorpt_correction_T_min  0.2025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1010 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.7843.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_recrystallization_method
'Grown from concentrated THF solution at 238K.'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.946
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1473
_refine_ls_number_reflns         18988
_refine_ls_number_restraints     472
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+39.4445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14263
_reflns_number_total             18988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           jfih980new_a
_cod_depositor_comments
'Adding full bibliography for 4086816--4086827.cif.'
_cod_database_code               4086822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3A-O4A = C4-O3 = C3-O4 = O3A-C4A = C70A-O7A
 1.17 with sigma of 0.02
 C69-O7
 1.3 with sigma of 0.02
 O2-C1
 1.26 with sigma of 0.02
 C67-O6
 1.26 with sigma of 0.02
 O8A-C68
 1.36 with sigma of 0.02
 C68-C67
 1.48 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C70A) = Uanis(O5)
Uanis(C4A) = Uanis(O2)
Uanis(O1A) = Uanis(C3)
Uanis(C69) = Uanis(O6A) = Uanis(O7)
Uanis(O1) = Uanis(C3A)
Uanis(O8A) = Uanis(C68)
4. Rigid body (RIGU) restrains
 Mn2A, O5A, O6A, O7A, O8A, C70A, C69A, C67A, C68A, Mn2, O7, O8, O5, O6, C69,
 C67, C70, C68, N4, C72, N3, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C6, N1, C5, Mn1A, O4, O2, O1, O3, C4, C2, C3, C1, Mn1, O1A, O2A, O4A, O3A,
  C1A, C2A, C4A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4)=Sof(O2)=Sof(O1)=Sof(O3)=Sof(C4)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=
 Sof(C3)=Sof(C1)=Sof(Mn1)=1-FVAR(1)
 Sof(Mn1A)=Sof(O1A)=Sof(O2A)=Sof(O4A)=Sof(O3A)=Sof(C1A)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=Sof(C4A)=Sof(C3A)=FVAR(1)
 Sof(Mn2)=Sof(O7)=Sof(O8)=Sof(O5)=Sof(O6)=Sof(C69)=Sof(C67)=Sof(C70)=Sof(C68)=
 Sof(H68D)=Sof(H68E)=Sof(H68F)=1-FVAR(2)
 Sof(Mn2A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(C70A)=Sof(C69A)=Sof(C67A)=
 Sof(C68A)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C88(H88), C115(H115), C130(H130), C85(H85), C97(H97), C119(H119), C127(H127),
 C100(H100), C61(H61), C64(H64), C52(H52), C49(H49), C31(H31), C34(H34),
 C19(H19), C22(H22)
6.b Aromatic/amide H refined with riding coordinates:
 C75(H75), C107(H107), C105(H105), C76(H76), C77(H77), C106(H106), C82(H82),
 C123(H123), C81(H81), C125(H125), C124(H124), C83(H83), C96(H96), C113(H113),
 C112(H112), C95(H95), C94(H94), C111(H111), C40(H40), C41(H41), C39(H39),
 C59(H59), C58(H58), C57(H57), C45(H45), C46(H46), C47(H47), C11(H11), C10(H10),
  C9(H9), C27(H27), C28(H28), C29(H29), C15(H15), C16(H16), C17(H17)
6.c Idealised Me refined as rotating group:
 C129(H12A,H12B,H12C), C90(H90A,H90B,H90C), C128(H12D,H12E,H12F), C98(H98A,
 H98B,H98C), C117(H11A,H11B,H11C), C89(H89A,H89B,H89C), C99(H99A,H99B,H99C),
 C118(H11D,H11E,H11F), C120(H12G,H12H,H12I), C131(H13A,H13B,H13C), C101(H10A,
 H10B,H10C), C132(H13D,H13E,H13F), C102(H10D,H10E,H10F), C116(H11G,H11H,H11I),
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C68A(H68A,H68B,H68C), C68(H68D,H68E,
 H68F), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C51(H51A,H51B,H51C),
 C50(H50A,H50B,H50C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              25307
_shelx_hkl_checksum              8396
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JFig980
_olex2_submission_special_instructions 'No special instructions were received'