Comparison of Nucleophilic- and Radical-Based Routes to the Formation of Manganese-Main Group Element Single Bonds
Figueroa, Joshua S.; Agnew, Douglas W.; Moore, Curtis E.; Rheingold, Arnold L.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01102D

data_7042717
_publ_section_title
;
 Comparison of Nucleophilic- and Radical-Based Routes to the Formation of
 Manganese-Main Group Element Single Bonds
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01102D
_journal_year                    2017
_chemical_formula_moiety         'C65 H74 F2 Mn N2 O3 Sb, 2(C5 H5 N)'
_chemical_formula_sum            'C75 H84 F2 Mn N4 O3 Sb'
_chemical_formula_weight         1304.15
_chemical_name_common            Mn(SbF2)(CO)3(CNArDipp2)2_2(pyr)
_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             2016-10-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.8090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9656(4)
_cell_length_b                   17.3952(4)
_cell_length_c                   25.1885(6)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.908
_cell_measurement_theta_min      2.217
_cell_volume                     6847.4(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55310
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.120
_diffrn_reflns_theta_min         1.303
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1079 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.9270. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_recrystallization_method
'Grown from saturated pyridine solution at -40C'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.672
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13552
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0678P)^2^+10.8995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10944
_reflns_number_total             13552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01102d2.cif
_cod_data_source_block           jfig1141
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7042717
_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(F2A) = Uanis(F1) = Uanis(F1A) = Uanis(F2)
Uanis(C16A) = Uanis(C16) = Uanis(C15) = Uanis(C15A)
3. Rigid body (RIGU) restrains
 C14S, N3S, C11S, C13S, C15S, C12S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7S, C8S, C9S, C10S, N2S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F2)=Sof(F1)=FVAR(1)
 Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(H14)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=FVAR(2)
 Sof(C7S)=Sof(H7S)=Sof(C8S)=Sof(H8S)=Sof(C9S)=Sof(H9S)=Sof(C10S)=Sof(H10S)=
 Sof(N2S)=Sof(C6S)=Sof(H6S)=1-FVAR(3)
 Sof(N3S)=Sof(C11S)=Sof(H11S)=Sof(C13S)=Sof(H13S)=Sof(C12S)=Sof(H12S)=
 Sof(C15S)=Sof(H15S)=Sof(C14S)=Sof(H14S)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C33(H33), C26(H26), C44(H44), C51(H51), C21(H21), C63(H63), C56(H56),
 C14(H14), C14(H14A)
5.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C40(H40), C10(H10), C9(H9), C38(H38), C8(H8), C61(H61), C59(H59),
 C30(H30), C29(H29), C60(H60), C31(H31), C17(H17), C18(H18), C47(H47), C49(H49),
  C19(H19), C5S(H5S), C48(H48), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S),
 C11S(H11S), C13S(H13S), C12S(H12S), C15S(H15S), C14S(H14S), C7S(H7S), C8S(H8S),
  C9S(H9S), C10S(H10S), C6S(H6S)
5.c Fitted hexagon refined as free rotating group:
 C7S(C8S,C9S,C10S,N2S,C6S)
5.d Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C53(H53A,H53B,H53C), C46(H46A,H46B,H46C), C65(H65A,H65B,
 H65C), C52(H52A,H52B,H52C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C28(H28A,
 H28B,H28C), C45(H45A,H45B,H45C), C58(H58A,H58B,H58C), C35(H35A,H35B,H35C),
 C57(H57A,H57B,H57C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C16(H16A,H16B,
 H16C), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              32700
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JFig1141
_olex2_submission_special_instructions 'No special instructions were received'