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_4086818
_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         'C72 H94 Mn N2 O4, C32 H12 B F24'
_chemical_formula_sum            'C104 H106 B F24 Mn N2 O4'
_chemical_formula_weight         1969.65
_chemical_name_systematic
;
 ?
;
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.988(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.384(3)
_cell_length_b                   16.256(2)
_cell_length_c                   49.409(6)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.266
_cell_measurement_theta_min      2.174
_cell_volume                     19944(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            127613
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        21.000
_diffrn_reflns_theta_max         21.000
_diffrn_reflns_theta_min         0.997
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.0412
_exptl_absorpt_correction_T_min  0.0215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1308 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.5218.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             8176
_exptl_crystal_recrystallization_method
'Grown from diethyl ether solution at 238K'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2577
_refine_ls_number_reflns         21546
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.1376
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+274.3766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3216
_refine_ls_wR_factor_ref         0.3348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17106
_reflns_number_total             21546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           JFig998
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086816--4086827.cif.
;
_cod_database_code               4086818
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9837(6) 0.0163(6)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C111)
Uanis(C1B) = Uanis(C110)
Uanis(F22) = Uanis(F23A)
4. Rigid body (RIGU) restrains
 F47A, F47, C208, F45, F45A, F46, F46A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F24A, C159, F22A, F23, F23A, F2AA, F22
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F21A, F21, C172, F19, F19A, F20, F20A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7, C6, O4, C5, C8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C79, C78, O011, C77, C80, C81, O8, C84, C83, C82
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C111, C1A, C109, C110, C1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F21A)=Sof(F20A)=Sof(F19A)=1-FVAR(1)
 Sof(F19)=Sof(F21)=Sof(F20)=FVAR(1)
 Sof(F47A)=Sof(F45A)=Sof(F46A)=1-FVAR(2)
 Sof(F47)=Sof(F45)=Sof(F46)=FVAR(2)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F2AA)=FVAR(3)
 Sof(H10D)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=
 Sof(H1BC)=1-FVAR(4)
 Sof(H109)=Sof(C111)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C110)=Sof(H11J)=
 Sof(H11K)=Sof(H11L)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C68(H68), C130(H130), C142(H142), C139(H139), C112(H112), C127(H127),
 C58(H58), C55(H55), C26(H26), C70(H70), C97(H97), C100(H100), C109(H109),
 C109(H10D), C37(H37), C40(H40), C29(H29)
6.b Secondary CH2 refined with riding coordinates:
 C77(H77A,H77B), C10(H10H,H10I), C9(H9A,H9B), C81(H81A,H81B), C84(H84A,H84B),
 C78(H78A,H78B), C5(H5A,H5B), C6(H6A,H6B)
6.c Aromatic/amide H refined with riding coordinates:
 C195(H195), C209(H209), C63(H63), C47(H47), C168(H168), C45(H45), C117(H117),
 C165(H165), C125(H125), C184(H184), C198(H198), C89(H89), C178(H178),
 C152(H152), C201(H201), C176(H176), C64(H64), C162(H162), C138(H138),
 C154(H154), C107(H107), C46(H46), C118(H118), C119(H119), C186(H186),
 C203(H203), C171(H171), C106(H106), C88(H88), C95(H95), C192(H192), C94(H94),
 C124(H124), C65(H65), C136(H136), C87(H87), C160(H160), C105(H105), C135(H135),
  C206(H206), C123(H123), C146(H146), C93(H93), C173(H173), C16(H16), C51(H51),
 C34(H34), C24(H24), C149(H149), C52(H52), C53(H53), C157(H157), C35(H35),
 C181(H181), C15(H15), C23(H23), C17(H17), C33(H33), C22(H22), C189(H189)
6.d Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C69(H69A,H69B,H69C), C67(H67A,H67B,H67C), C132(H13A,
 H13B,H13C), C141(H14A,H14B,H14C), C140(H14D,H14E,H14F), C114(H11A,H11B,H11C),
 C143(H14G,H14H,H14I), C101(H10E,H10F,H10G), C59(H59A,H59B,H59C), C38(H38A,H38B,
 H38C), C60(H60A,H60B,H60C), C57(H57A,H57B,H57C), C144(H14J,H14K,H14L),
 C71(H71A,H71B,H71C), C56(H56A,H56B,H56C), C41(H41A,H41B,H41C), C131(H13D,H13E,
 H13F), C28(H28A,H28B,H28C), C128(H12A,H12B,H12C), C39(H39A,H39B,H39C),
 C72(H72A,H72B,H72C), C31(H31A,H31B,H31C), C113(H11D,H11E,H11F), C129(H12D,H12E,
 H12F), C111(H11G,H11H,H11I), C27(H27A,H27B,H27C), C80(H80A,H80B,H80C),
 C12(H12G,H12H,H12I), C42(H42A,H42B,H42C), C30(H30A,H30B,H30C), C98(H98A,H98B,
 H98C), C99(H99A,H99B,H99C), C83(H83A,H83B,H83C), C110(H11J,H11K,H11L),
 C11(H11M,H11N,H11O), C82(H82A,H82B,H82C), C79(H79A,H79B,H79C), C7(H7A,H7B,H7C),
  C8(H8A,H8B,H8C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              84340
_shelx_hkl_checksum              24894
_shelx_shelxl_version_number     2016/5
_olex2_submission_original_sample_id JFig998
_olex2_submission_special_instructions 'No special instructions were received'