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_4086827
_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         'C71 H79 Mn N2 O4, C3 H3'
_chemical_formula_sum            'C74 H82 Mn N2 O4'
_chemical_formula_weight         1118.35
_chemical_name_common            Mn(k2-benzoate)CO2(CNArDipp2)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.2914(10)
_cell_length_b                   16.5737(4)
_cell_length_c                   16.9876(4)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.41
_cell_volume                     12594.4(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_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 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41563
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_min         1.310
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.4545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1161 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.9274.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       plate
_exptl_crystal_F_000             4776
_exptl_crystal_recrystallization_method
'Grown from benzene/Et2O mixture at room temperature over 24 h'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         11494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0340P)^2^+15.8120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8503
_reflns_number_total             11494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           jfig1408
_cod_depositor_comments
'Adding full bibliography for 4086816--4086827.cif.'
_cod_database_code               4086827
_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.a Ternary CH refined with riding coordinates:
 C57(H57), C69(H69), C66(H66), C54(H54), C28(H28), C24(H24), C39(H39), C36(H36)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C44(H44), C45(H45), C51(H51), C50(H50), C16(H16), C15(H15),
 C14(H14), C64(H64), C22(H22), C21(H21), C62(H62), C52(H52), C20(H20), C34(H34),
  C63(H63), C32(H32), C33(H33), C11(H11), C10(H10), C1S(H1S), C7(H7), C2S(H2S),
 C3S(H3S), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C59(H59A,H59B,H59C), C58(H58A,H58B,H58C), C25(H25A,H25B,
 H25C), C68(H68A,H68B,H68C), C27(H27A,H27B,H27C), C71(H71A,H71B,H71C), C70(H70A,
 H70B,H70C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C), C41(H41A,H41B,H41C),
 C55(H55A,H55B,H55C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C29(H29A,H29B,
 H29C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              48782
_shelx_hkl_checksum              84372
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JFig1408
_olex2_submission_special_instructions 'No special instructions were received'