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_4086826
_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         '0.5(C136 H168 K2 Mn2 N4 O6)'
_chemical_formula_sum            'C68 H84 K Mn N2 O3'
_chemical_formula_weight         1071.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 104.977(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.142(5)
_cell_length_b                   27.610(8)
_cell_length_c                   27.492(8)
_cell_measurement_reflns_used    4774
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      20.753
_cell_measurement_theta_min      2.322
_cell_volume                     14036(7)
_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 0.997
_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  0.0959
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.865
_diffrn_reflns_theta_max         20.865
_diffrn_reflns_theta_min         1.064
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.0854
_exptl_absorpt_correction_T_min  0.0547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1181 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.6405.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_description       block
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1428
_refine_ls_number_reflns         14754
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0767P)^2^+56.6878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9923
_reflns_number_total             14754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           JFig1036
_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_cell_volume        14037(7)
_cod_database_code               4086826
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.983
_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. Restrained distances
 O1S'-C3S'
 1.4 with sigma of 0.02
 O1S'-C2S'
 1.4 with sigma of 0.02
 C2S'-C1S'
 1.5 with sigma of 0.02
 C3S'-C4S'
 1.5 with sigma of 0.02
 O1B-C2B = O1B-C3B
 1.4 with sigma of 0.02
 C1B-C2B = C4B-C3B
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1B) = Uanis(O1S')
4. Rigid body (RIGU) restrains
 K1', O1S', O1B, C1S', C2S', C3S', C4S', C1B, C2B, C3B, C4B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O1S'(0.5) O1B(0.5) C1S'(0.5) H1SD(0.5) H1SE(0.5) H1SF(0.5)
 C2S'(0.5) H2SC(0.5) H2SD(0.5) C3S'(0.5) H3SC(0.5) H3SD(0.5) C4S'(0.5)
 H4SD(0.5) H4SE(0.5) H4SF(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C2B(0.5)
 H2BA(0.5) H2BB(0.5) C3B(0.5) H3BA(0.5) H3BB(0.5) C4B(0.5) H4BA(0.5) H4BB(0.5)
 H4BC(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C17(H17), C20(H20), C29(H29), C32(H32), C47(H47), C50(H50),
 C59(H59), C62(H62), C7'(H7'), C8'(H8'), C17'(H17'), C20'(H20'), C29'(H29'),
 C32'(H32'), C47'(H47'), C50'(H50'), C59'(H59'), C62'(H62')
6.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C2S'(H2SC,H2SD), C3S'(H3SC,H3SD), C2B(H2BA,
 H2BB), C3B(H3BA,H3BB)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C15(H15), C16(H16), C25(H25), C26(H26), C27(H27), C37(H37),
 C38(H38), C39(H39), C43(H43), C44(H44), C45(H45), C55(H55), C56(H56), C57(H57),
  C6'(H6'), C14'(H14'), C15'(H15'), C16'(H16'), C25'(H25'), C26'(H26'),
 C27'(H27'), C37'(H37'), C38'(H38'), C39'(H39'), C43'(H43'), C44'(H44'),
 C45'(H45'), C55'(H55'), C56'(H56'), C57'(H57')
6.d Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C60(H60A,H60B,
 H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C18'(H18D,H18E,H18F), C19'(H19D,H19E,H19F), C21'(H21D,H21E,H21F), C22'(H22D,
 H22E,H22F), C30'(H30D,H30E,H30F), C31'(H31D,H31E,H31F), C33'(H33D,H33E,H33F),
 C34'(H34D,H34E,H34F), C48'(H48D,H48E,H48F), C49'(H49D,H49E,H49F), C51'(H51D,
 H51E,H51F), C52'(H52D,H52E,H52F), C60'(H60D,H60E,H60F), C61'(H61D,H61E,H61F),
 C63'(H63D,H63E,H63F), C64'(H64D,H64E,H64F), C1S'(H1SD,H1SE,H1SF), C4S'(H4SD,
 H4SE,H4SF), C1B(H1BA,H1BB,H1BC), C4B(H4BA,H4BB,H4BC)
;
_shelx_res_checksum              59853
_shelx_hkl_checksum              73563
_shelx_fab_checksum              23212
_shelx_shelxl_version_number     2016/5
_olex2_submission_special_instructions 'No special instructions were received'