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_7042716
_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 Bi Cl2 Mn N2 O3, C4 H8 O, C4 H7 O'
_chemical_formula_sum            'C73 H89 Bi Cl2 Mn N2 O5'
_chemical_formula_weight         1409.28
_chemical_name_common            Mn(BiCl2)(CO)3(CNArDipp2)2
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0881(10)
_cell_length_b                   16.5315(9)
_cell_length_c                   24.8358(14)
_cell_measurement_reflns_used    7709
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.370
_cell_measurement_theta_min      2.353
_cell_volume                     6765.2(7)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40804
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.450
_diffrn_reflns_theta_min         1.236
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.913
_exptl_absorpt_correction_T_max  0.0186
_exptl_absorpt_correction_T_min  0.0056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0832 before and 0.0511 after correction. The Ratio of minimum to maximum transmission is 0.3011. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2892
_exptl_crystal_recrystallization_method
'grown from saturated THF solution at -40C'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.586
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         12473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0612
_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^)+(0.1098P)^2^+15.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9740
_reflns_number_total             12473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01102d2.cif
_cod_data_source_block           jfig947_new_a
_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               7042716
_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.a Ternary CH refined with riding coordinates:
 C60(H60), C30(H30), C63(H63), C33(H33), C51(H51), C18(H18), C21(H21), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C4S(H4SA,H4SB), C3S(H3SA,H3SB), C6S(H6SA,H6SB), C5S(H5SA,
 H5SB), C7S(H7SA,H7SB), C2S(H2SA,H2SB)
2.c Aromatic/amide H refined with riding coordinates:
 C56(H56), C10(H10), C39(H39), C28(H28), C46(H46), C58(H58), C38(H38),
 C27(H27), C44(H44), C9(H9), C26(H26), C8(H8), C45(H45), C40(H40), C57(H57),
 C14(H14), C16(H16), C15(H15), C8S(H8S)
2.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C31(H31A,H31B,H31C), C62(H62A,H62B,H62C), C53(H53A,H53B,
 H53C), C65(H65A,H65B,H65C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C52(H52A,
 H52B,H52C), C35(H35A,H35B,H35C), C64(H64A,H64B,H64C), C34(H34A,H34B,H34C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C50(H50A,H50B,
 H50C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              26628
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id JFig947
_olex2_submission_special_instructions 'No special instructions were received'