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_7042718
_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 H74.57 F1.57 Mn N2 O3, 0.43(F), C2 H5 O0.47'
_chemical_formula_sum            'C67 H79.57 F2 Mn N2 O3.47'
_chemical_formula_weight         1061.27
_chemical_name_common            Mn(FHF)(CO)3(CNArDipp2)
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1678(5)
_cell_length_b                   16.5149(4)
_cell_length_c                   20.6165(5)
_cell_measurement_reflns_used    3483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      3.78
_cell_volume                     5957.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.9-0 (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    '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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46752
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.284
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker MicroStar FR-592'
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  0.5210
_exptl_absorpt_correction_T_min  0.4202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             2265
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         10877
_refine_ls_number_restraints     654
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0702P)^2^+3.8567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9629
_reflns_number_total             10877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01102d2.cif
_cod_data_source_block           jfigcu128
_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               7042718
_shelx_shelxl_version_number     2016/6
_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(C6) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C1S2) = Uanis(C1S)
Uanis(C2S2) = Uanis(C2S)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(C2S)=Sof(H2SD)=Sof(H2SE)=Sof(H2SF)=1-FVAR(1)
 Sof(C1S2)=Sof(H1SA)=Sof(H1SB)=Sof(C2S2)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=FVAR(1)
 Sof(F4)=Sof(H4)=Sof(F2)=Sof(O4)=Sof(C5)=1-FVAR(2)
 Sof(F1)=Sof(F3)=Sof(O3)=Sof(C6)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C27(H27), C34(H34), C45(H45), C52(H52), C57(H57), C64(H64)
5.b Secondary CH2 refined with riding coordinates:
 C1S2(H1SA,H1SB), C1S(H1SC,H1SD)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17), C30(H30), C31(H31),
 C32(H32), C39(H39), C40(H40), C41(H41), C48(H48), C49(H49), C51(H51), C60(H60),
  C61(H61), C62(H62)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C2S2(H2SA,H2SB,H2SC), C2S(H2SD,H2SE,H2SF)
;
_shelx_res_checksum              87331
_olex2_submission_original_sample_id JFigCu128
_olex2_submission_special_instructions 'No special instructions were received'