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_4086819
_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         'C67 H74 F3 Mn N2 O5, C2 H5 O0.5'
_chemical_formula_sum            'C69 H79 F3 Mn N2 O5.5'
_chemical_formula_weight         1136.28
_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     direct
_audit_creation_date             2016-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.2250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5450(4)
_cell_length_b                   16.6493(3)
_cell_length_c                   20.6945(4)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.45
_cell_volume                     6294.6(2)
_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      100.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.979
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65026
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_min         2.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_recrystallization_method
'grown from concentrated et2o solution at -40C'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         12643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0561P)^2^+4.1395P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10680
_reflns_number_total             12643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           jfig1020
_cod_depositor_comments
'Adding full bibliography for 4086816--4086827.cif.'
_cod_original_cell_volume        6294.5(2)
_cod_original_formula_sum        'C69 H79 F3 Mn N2 O5.50'
_cod_database_code               4086819
_shelxl_version_number           2013-2
_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, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H49A)=Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C50)=Sof(H50D)=
 Sof(H50E)=Sof(H50F)=1-FVAR(1)
 Sof(H49)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C50A)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(O4A)=Sof(O5A)=Sof(C1A)=Sof(F3A)=1-FVAR(2)
 Sof(O4)=Sof(O5)=Sof(C1)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Sof(H61A)=Sof(C63)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C62)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=1-FVAR(3)
 Sof(H61)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63A)=Sof(H63A)=
 Sof(H63B)=Sof(H63C)=FVAR(3)
 Fixed Sof: H1SD(0.5) H1SE(0.5) H1SF(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5)
 C3S(0.5) H3SA(0.5) H3SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
3.a Ternary CH refined with riding coordinates:
 C31(H31), C28(H28), C19(H19), C0AA(H0AA), C46(H46), C49(H49), C49(H49A),
 C58(H58), C61(H61), C61(H61A)
3.b Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C2S(H2SA,H2SB)
3.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C24(H24), C9(H9), C10(H10), C11(H11), C17(H17), C16(H16),
 C15(H15), C42(H42), C43(H43), C44(H44), C36(H36), C37(H37), C38(H38), C54(H54),
  C55(H55), C56(H56)
3.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC),
 C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C50A(H50A,H50B,
 H50C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62A(H62A,H62B,H62C),
 C63A(H63A,H63B,H63C), C30(H30A,H30B,H30C), C51A(H51D,H51E,H51F), C50(H50D,H50E,
 H50F), C1S(H1SD,H1SE,H1SF), C1S(H1SA,H1SB,H1SC), C63(H63D,H63E,H63F), C62(H62D,
 H62E,H62F)
;
_shelx_res_checksum              90262
_shelx_hkl_checksum              78501
_olex2_submission_original_sample_id JFig1020
_olex2_submission_special_instructions 'No special instructions were received'