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_4086817
_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         'C70 H80 Mn N3 O4, 2(C4 H10 O)'
_chemical_formula_sum            'C78 H100 Mn N3 O6'
_chemical_formula_weight         1230.54
_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             2016-06-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7361(3)
_cell_length_b                   17.6996(3)
_cell_length_c                   26.0679(5)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.17
_cell_volume                     7084.6(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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49983
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.776
_diffrn_reflns_theta_max         24.776
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.2582
_exptl_absorpt_correction_T_min  0.2261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.8757.
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    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_recrystallization_method
'Grown from diethyl ether/pyridine solution at 238K.'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.263
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         12137
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0892
_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^)+(0.0987P)^2^+17.3160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9791
_reflns_number_total             12137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           jfig982_new_a
_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               4086817
_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. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C1)
3. Rigid body (RIGU) restrains
 N3, C4, N1, C5, Mn1, N2, C6, C10, C7, C8, C9, O1, O2, O3A, C1, C2A, C3, O2A,
 C1A, O1A, O3, C2, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H53A)=Sof(C55)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C54)=Sof(H54D)=Sof(H54E)=
 Sof(H54F)=1-FVAR(1)
 Sof(H53)=Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C54A)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=FVAR(1)
 Sof(O2A)=Sof(C1A)=Sof(H1A)=Sof(O1A)=Sof(O3A)=Sof(C2A)=1-FVAR(2)
 Sof(O1)=Sof(O2)=Sof(C1)=Sof(H1)=Sof(O3)=Sof(C2)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C65(H65), C23(H23), C36(H36), C01D(H01D), C53(H53), C53(H53A),
 C50(H50), C62(H62)
5.b Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C2S(H2SA,H2SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C40(H40), C42(H42), C21(H21), C20(H20),
 C19(H19), C41(H41), C6(H6), C58(H58), C47(H47), C46(H46), C48(H48), C59(H59),
 C60(H60), C10(H10), C33(H33), C7(H7), C31(H31), C8(H8), C9(H9), C32(H32),
 C1A(H1A), C1(H1)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C01L(H01A,H01B,
 H01C), C25(H25A,H25B,H25C), C67(H67A,H67B,H67C), C24(H24A,H24B,H24C), C66(H66A,
 H66B,H66C), C52(H52A,H52B,H52C), C35(H35A,H35B,H35C), C64(H64A,H64B,H64C),
 C51(H51A,H51B,H51C), C63(H63A,H63B,H63C), C028(H02A,H02B,H02C), C55A(H55A,H55B,
 H55C), C54A(H54A,H54B,H54C), C55(H55D,H55E,H55F), C54(H54D,H54E,H54F),
 C8S(H8SA,H8SB,H8SC), C5S(H5SA,H5SB,H5SC), C4S(H4SA,H4SB,H4SC), C1S(H1SA,H1SB,
 H1SC)
;
_shelx_res_checksum              27480
_shelx_hkl_checksum              31178
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JFig982
_olex2_submission_special_instructions 'No special instructions were received'