Interconversion and reactivity of manganese silyl, silylene, and silene complexes
Price, Jeffrey S.; Emslie, David J. H.; Chemical Science  (2019) –; doi:10.1039/C9SC04513A

data_1552513
_publ_section_title
;
 Interconversion and reactivity of manganese silyl, silylene, and silene
 complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC04513A
_journal_year                    2019
_chemical_formula_moiety         'C27 H48 Mn N P4 Si'
_chemical_formula_sum            'C27 H48 Mn N P4 Si'
_chemical_formula_weight         593.57
_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     dual
_audit_creation_date             2019-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-09 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.7800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0996(2)
_cell_length_b                   18.7393(4)
_cell_length_c                   15.7941(4)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.917
_cell_measurement_theta_min      2.276
_cell_volume                     3145.27(12)
_computing_cell_refinement       'SAINT v8.34A (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78139
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.178
_diffrn_reflns_theta_min         1.730
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  
 'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0450 before and 0.0376 after correction.
The Ratio of minimum to maximum transmission is 0.9172.
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         11961
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+1.1098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9601
_reflns_number_total             11961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04513a3.cif
_cod_data_source_block           MnHSiPh_xylylNC
_cod_database_code               1552513
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.773
_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. Shared sites
{P3, P4A}
{P1, P1A}
3. Restrained distances
 P4-Mn1 \\sim Mn1-P2A
 with sigma of 0.005
 P3A-Mn1 \\sim Mn1-P2
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(P3A) = Uanis(P2)
Uanis(P4) = Uanis(P2A)
Uanis(C27) = Uanis(C21A)
Uanis(C18A) = Uanis(C16)
Uanis(C16A) = Uanis(C17)
Uanis(C18) = Uanis(C17A)
Uanis(C23) = Uanis(C25A)
Uanis(C19A) = Uanis(C27)
Uanis(C21) = Uanis(C24A)
Uanis(C21) = Uanis(C23A)
Uanis(C20) = Uanis(C22A)
Uanis(C24) = Uanis(C26A)
Uanis(C27A) = Uanis(C22)
Uanis(C26) = Uanis(C20A)
Uanis(P3) = Uanis(P4A)
Uanis(P1) = Uanis(P1A)
5. Same fragment restrains
{P1, P2, C16, C17, C18, C19, C20, C21} sigma for 1-2: 0.002, 1-3: 0.004
as
{P3, P4, C22, C23, C24, C25, C26, C27}
{P1, P2, C16, C17, C18, C19, C20, C21} sigma for 1-2: 0.002, 1-3: 0.004
as
{P1A, P2A, C16A, C17A, C18A, C19A, C20A, C21A}
{P1, P2, C16, C17, C18, C19, C20, C21} sigma for 1-2: 0.002, 1-3: 0.004
as
{P3A, P4A, C22A, C23A, C24A, C25A, C26A, C27A}
6. Others
 Sof(P1A)=Sof(P2A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=
 Sof(H19D)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(P3A)=Sof(P4A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24C)=Sof(H24D)=
 Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(P1)=Sof(P2)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(P3)=Sof(P4)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C24(H24A,H24B), C25(H25A,H25B), C18A(H18C,
 H18D), C19A(H19C,H19D), C24A(H24C,H24D), C25A(H25C,H25D)
7.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C27(H27A,H27B,
 H27C), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C23A(H23D,H23E,H23F),
 C26A(H26D,H26E,H26F)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C),
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C20A(H20D,H20E,H20F), C21A(H21D,H21E,
 H21F), C22A(H22D,H22E,H22F), C27A(H27D,H27E,H27F)
;
_shelx_res_checksum              4180
_olex2_submission_special_instructions 'No special instructions were received'