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_4086825
_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         'C87 H83 B F15 Mn N2 O4, 0.5(C4 H10 O)'
_chemical_formula_sum            'C89 H88 B F15 Mn N2 O4.5'
_chemical_formula_weight         1608.36
_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   mixed
_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                97.8460(10)
_cell_angle_beta                 98.6420(10)
_cell_angle_gamma                90.6020(10)
_cell_formula_units_Z            4
_cell_length_a                   14.7941(8)
_cell_length_b                   24.7433(13)
_cell_length_c                   26.5070(14)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.052
_cell_measurement_theta_min      2.268
_cell_volume                     9498.3(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II TXS'
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            141336
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.449
_diffrn_reflns_theta_min         1.569
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.0917
_exptl_absorpt_correction_T_min  0.0669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1053 before and 0.0407 after correction.
The Ratio of minimum to maximum transmission is 0.7296.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2119
_refine_ls_number_reflns         35043
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+4.8339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26288
_reflns_number_total             35043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           JFig1104
_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_original_formula_sum        'C89 H88 B F15 Mn N2 O4.50'
_cod_database_code               4086825
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.979
_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. Rigid body (RIGU) restrains
 C92, C93, C95A, C95, C96A, C96, C94A, C94
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(C94)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=Sof(C95)=Sof(H95A)=Sof(H95B)=
 Sof(H95C)=Sof(H94A)=Sof(H94B)=Sof(H94C)=1-FVAR(1)
 Sof(C95A)=Sof(H95D)=Sof(H95E)=Sof(H95F)=Sof(C96A)=Sof(H96D)=Sof(H96E)=
 Sof(H96F)=Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C73(H73), C70(H70), C139(H139), C171(H171), C130(H130), C82(H82), C168(H168),
 C158(H158), C127(H127), C153(H153), C142(H142), C85(H85), C40(H40), C55(H55),
 C43(H43), C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C3S(H3SA,H3SB)
4.c Aromatic/amide H refined with riding coordinates:
 C119(H119), C117(H117), C61(H61), C60(H60), C62(H62), C68(H68), C118(H118),
 C147(H147), C149(H149), C66(H66), C67(H67), C137(H137), C148(H148), C123(H123),
  C157(H157), C80(H80), C125(H125), C79(H79), C136(H136), C32(H32), C78(H78),
 C156(H156), C124(H124), C135(H135), C166(H166), C30(H30), C164(H164), C31(H31),
  C36(H36), C155(H155), C38(H38), C48(H48), C37(H37), C165(H165), C49(H49),
 C50(H50)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C),
 C74(H74A,H74B,H74C), C140(H14A,H14B,H14C), C71(H71A,H71B,H71C), C173(H17A,H17B,
 H17C), C84(H84A,H84B,H84C), C83(H83A,H83B,H83C), C161(H16A,H16B,H16C),
 C172(H17D,H17E,H17F), C132(H13A,H13B,H13C), C141(H14D,H14E,H14F), C055(H05A,
 H05B,H05C), C41(H41A,H41B,H41C), C143(H14G,H14H,H14I), C169(H16D,H16E,H16F),
 C160(H16G,H16H,H16I), C131(H13D,H13E,H13F), C96(H96A,H96B,H96C), C95(H95A,H95B,
 H95C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C154(H15A,H15B,H15C),
 C42(H42A,H42B,H42C), C129(H12A,H12B,H12C), C144(H14J,H14K,H14L), C128(H12D,
 H12E,H12F), C45(H45A,H45B,H45C), C57(H57A,H57B,H57C), C44(H44A,H44B,H44C),
 C170(H17G,H17H,H17I), C56(H56A,H56B,H56C), C54(H54A,H54B,H54C), C2S(H2SA,H2SB,
 H2SC), C4S(H4SA,H4SB,H4SC), C53(H53A,H53B,H53C), C95A(H95D,H95E,H95F),
 C96A(H96D,H96E,H96F), C94A(H94D,H94E,H94F)
;
_shelx_res_checksum              21515
_shelx_hkl_checksum              95837
_shelx_fab_checksum              50214
_shelx_shelxl_version_number     2016/5
_olex2_submission_special_instructions 'No special instructions were received'