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_4086823
_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 H79 Mn N2 O5, 2(C4 H10 O)'
_chemical_formula_sum            'C80 H99 Mn N2 O7'
_chemical_formula_weight         1255.55
_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   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                97.684(4)
_cell_angle_beta                 91.435(4)
_cell_angle_gamma                96.967(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2792(15)
_cell_length_b                   16.609(2)
_cell_length_c                   19.630(3)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.198
_cell_measurement_theta_min      2.267
_cell_volume                     3934.7(9)
_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                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70456
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.440
_diffrn_reflns_theta_min         2.171
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0642 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.7249.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       Block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         14439
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0656P)^2^+0.6511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9180
_reflns_number_total             14439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           JFig902
_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.

'_exptl_crystal_colour_primary' value 'Yellow' changed to 'yellow'
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_cell_volume        3934.6(9)
_cod_database_code               4086823
_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
 O4, O5, O4A, O5A, C6, C7, C8, C9, C10, C11, C12, C6A, C7A, C8A, C9A, C10A,
 C11A, C12A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(O4)=Sof(O5)=Sof(C6)=1-FVAR(1)
 Sof(O4A)=Sof(O5A)=Sof(C6A)=FVAR(1)
 Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=1-FVAR(2)
 Sof(C7A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=
 Sof(H9A)=Sof(C8A)=Sof(H8A)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C37(H37), C40(H40), C55(H55), C58(H58), C67(H67), C70(H70)
4.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C33(H33),
 C34(H34), C35(H35), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C63(H63), C64(H64), C65(H65), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C8A(H8A)
4.d Fitted hexagon refined as free rotating group:
 C7A(C12A,C11A,C10A,C9A,C8A)
4.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC), C5S(H5SA,
 H5SB,H5SC), C8S(H8SA,H8SB,H8SC)
;
_shelx_res_checksum              24583
_shelx_hkl_checksum              47427
_shelx_fab_checksum              33733
_shelx_shelxl_version_number     2016/5
_olex2_submission_special_instructions 'No special instructions were received'