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_4086824
_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         'C69 H82.47 F3 Mn N2 O6 S, C4 H10 O'
_chemical_formula_sum            'C73 H92.47 F3 Mn N2 O7 S'
_chemical_formula_weight         1253.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 96.7370(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5867(17)
_cell_length_b                   15.1995(13)
_cell_length_c                   23.5502(17)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.355
_cell_measurement_theta_min      2.679
_cell_volume                     6962.7(10)
_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
_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 0.998
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28635
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.387
_diffrn_reflns_theta_min         3.197
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8620.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       Block
_exptl_crystal_F_000             2674
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.106(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         13378
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0504P)^2^+1.9566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12629
_reflns_number_total             13378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           JFig990
_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 'Red' changed to 'red'
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               4086824
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.894(13) 0.106(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S1AB-C1AB
 1.8 with sigma of 0.01
 F2AB-C1AB = F1AB-C1AB = F3AB-C1AB
 1.33 with sigma of 0.02
 F2AB-F3AB
 2.17 with sigma of 0.02
 F3AB-F1AB
 2.17 with sigma of 0.02
 F2AB-F1AB
 2.17 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C2S) = Uanis(C2SB)
Uanis(C3SB) = Uanis(C3S)
Uanis(C61) = Uanis(C61B)
Uanis(C59) = Uanis(C59B)
Uanis(S1A) = Uanis(S1AB)
Uanis(F2A) = Uanis(F2AB)
Uanis(F3A) = Uanis(F3AB)
Uanis(C60) = Uanis(C60A)
Uanis(O3AB) = Uanis(O3A)
5. Rigid body (RIGU) restrains
 S1AB, S1A, C1AB, C1A, F1A, F2AB, F2A, F3AB, F3A, F1AB, O3AB
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(S1AB)=Sof(F1AB)=Sof(F2AB)=Sof(F3AB)=Sof(O3AB)=Sof(H4SC)=Sof(H4SD)=
 Sof(C1AB)=1-FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O3A)=Sof(H4SA)=Sof(H4SB)=Sof(C1A)=
 FVAR(1)
 Sof(H1SC)=Sof(H1SD)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=Sof(H2SE)=Sof(C3SB)=
 Sof(H3SC)=Sof(H3SD)=Sof(H3SE)=1-FVAR(2)
 Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=
 FVAR(2)
 Sof(C59B)=Sof(H59B)=Sof(C61B)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(3)
 Sof(C59)=Sof(H59)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(3)
 Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(4)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C29(H29), C32(H32), C47(H47), C50(H50), C62(H62),
 C59(H59), C59B(H59B)
7.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1S(H1SC,H1SD), C4S(H4SA,H4SB), C4S(H4SC,H4SD), C2S(H2SA,
 H2SB), C3S(H3SA,H3SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB)
7.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C25(H25), C26(H26),
 C27(H27), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45), C55(H55),
  C56(H56), C57(H57)
7.d Idealised Me refined as rotating group:
 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), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C61(H61A,H61B,H61C), C2SB(H2SC,H2SD,H2SE), C3SB(H3SC,H3SD,H3SE),
 C61B(H61D,H61E,H61F), C5S(H5SA,H5SB,H5SC), C8S(H8SA,H8SB,H8SC), C60A(H60D,H60E,
 H60F)
;
_shelx_res_checksum              36363
_shelx_hkl_checksum              46351
_shelx_shelxl_version_number     2016/5
_olex2_submission_special_instructions 'No special instructions were received'