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_4086820
_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         'C65 H77 B F3 Mn N2 O5 S'
_chemical_formula_sum            'C65 H77 B F3 Mn N2 O5 S'
_chemical_formula_weight         1121.09
_chemical_name_common            (k2-F3CSO3BH3)-Mn(CO)2(CNArDipp2)2
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-09-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.025(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1452(7)
_cell_length_b                   15.6184(9)
_cell_length_c                   15.2093(7)
_cell_measurement_reflns_used    7190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.38
_cell_volume                     3118.2(3)
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19855
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.392
_diffrn_reflns_theta_min         2.103
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0616 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.8309.
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    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_recrystallization_method 'from concentrated et2o at 238K'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 3592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         10877
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+0.7846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.836
_reflns_Friedel_fraction_max     0.893
_reflns_number_gt                9216
_reflns_number_total             10877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00792_si_002.cif
_cod_data_source_block           jfig1145_0m_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               4086820
_shelxl_version_number           2014-3
_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(C50A) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) = Uanis(O4A)
Uanis(O5) = Uanis(O5A)
Uanis(B1A) = Uanis(B1)
Uanis(C50A) = Uanis(C50)
3. Rigid body (RIGU) restrains
 C50A, C48, C49, C47, C42, C43, C44, C45, C46, C51, C52, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S1A)=Sof(O4A)=Sof(O3A)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O5A)=Sof(B1A)=1-FVAR(1)
 Sof(S1)=Sof(O5)=Sof(F3A)=Sof(F1A)=Sof(O3)=Sof(F2A)=Sof(O4)=Sof(B1)=FVAR(1)
 Sof(H48A)=Sof(C50)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(2)
 Sof(H48)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C60(H60), C30(H30), C51(H51), C33(H33), C64(H64), C48(H48),
 C48(H48A), C21(H21)
5.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C58(H58), C28(H28), C8(H8), C10(H10), C40(H40), C26(H26), C9(H9),
 C57(H57), C39(H39), C46(H46), C16(H16), C56(H56), C44(H44), C45(H45), C27(H27),
  C15(H15), C14(H14)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C20(H20A,H20B,H20C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C65(H65A,H65B,H65C), C34(H34A,H34B,H34C), C23(H23A,H23B,H23C),
 C49(H49A,H49B,H49C), C35(H35A,H35B,H35C), C22(H22A,H22B,H22C), C63(H63A,H63B,
 H63C), C50A(H50A,H50B,H50C), C50(H50D,H50E,H50F)
;
_shelx_res_checksum              81943
_shelx_hkl_checksum              80254
_olex2_submission_original_sample_id JFig1145
_olex2_submission_special_instructions 'No special instructions were received'