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_7042715
_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         'C69 H82 Al Cl2 Mn N2 O4'
_chemical_formula_sum            'C69 H82 Al Cl2 Mn N2 O4'
_chemical_formula_weight         1156.18
_chemical_name_common            Mn(THF)(ALCl2)(CO)3(CNArDipp2)2
_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     iterative
_audit_creation_date             2017-02-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8827(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6958(5)
_cell_length_b                   26.0232(9)
_cell_length_c                   18.4253(6)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      2.22
_cell_volume                     6532.4(4)
_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    '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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36803
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.141
_diffrn_reflns_theta_max         24.141
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0599 before and 0.0524 after correction. The Ratio of minimum to maximum transmission is 0.8765. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         10356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0340P)^2^+9.5350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7960
_reflns_number_total             10356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01102d2.cif
_cod_data_source_block           jfig1032
_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               7042715
_shelx_shelxl_version_number     2014/7
_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. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C54(H54), C25(H25), C51(H51), C34(H34), C22(H22), C67(H67), C63(H63), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C48(H48), C18(H18), C49(H49), C43(H43), C47(H47), C12(H12),
 C32(H32), C42(H42), C41(H41), C13(H13), C20(H20), C61(H61), C31(H31), C59(H59),
  C60(H60), C30(H30)
3.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C64(H64A,H64B,H64C), C55(H55A,H55B,H55C), C52(H52A,H52B,
 H52C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C66(H66A,
 H66B,H66C), C65(H65A,H65B,H65C), C35(H35A,H35B,H35C), C56(H56A,H56B,H56C),
 C38(H38A,H38B,H38C), C69(H69A,H69B,H69C), C37(H37A,H37B,H37C), C24(H24A,H24B,
 H24C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              83829
_olex2_submission_original_sample_id JFig1032
_olex2_submission_special_instructions 'No special instructions were received'