Light- or oxidation-triggered CO release from [Mn(I)(CO)3(κ(3)-L)] complexes: reaction intermediates and a new synthetic route to [Mn(μ-O)2(L)2] compounds.
Sachs, Ulf; Schaper, Gerrit; Winkler, Daniela; Kratzert, Daniel; Kurz, Philipp; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17464–17473; doi:10.1039/c6dt02020h

data_7040834
_publ_section_title
;
 Light- or oxidation-triggered CO release from [Mn(I)(CO)3(\k(3)-L)]
 complexes: reaction intermediates and a new synthetic route to
 [Mn(\m-O)2(L)2] compounds.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17464
_journal_page_last               17473
_journal_paper_doi               10.1039/c6dt02020h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C18 H18 Mn N4 O), 3(F6 P1), C2 H3 N'
_chemical_formula_sum            'C38 H39 F18 Mn2 N9 O2 P3'
_chemical_formula_weight         1198.57
_chemical_name_common
bis(tris(2-pyridylmethyl)amine)bis(oxido)-bismanganese-tris(hexafluorophosphate)
_chemical_name_systematic
bis(tris(2-pyridylmethyl)amine)bis(oxido)-bismanganese-tris(hexafluorophosphate)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.445(7)
_cell_angle_beta                 86.987(7)
_cell_angle_gamma                66.838(7)
_cell_formula_units_Z            2
_cell_length_a                   10.2106(15)
_cell_length_b                   12.3868(19)
_cell_length_c                   19.944(3)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.21
_cell_volume                     2311.2(6)
_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      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82416
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.737
_diffrn_reflns_theta_min         1.024
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1144 before and 0.0498 after correction. The Ratio of minimum to maximum transmission is 0.9209. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear brownish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       plate
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14279
_refine_ls_number_restraints     782
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0510P)^2^+1.1887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10645
_reflns_number_total             14279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02020h3.cif
_cod_data_source_block           p-1_a
_cod_depositor_comments
'Adding full bibliography for 7040830--7040834.cif.'
_cod_database_code               7040834
_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. Restrained distances
 N1-C1 \\sim N1-C1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1B \\sim N2B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim
C1 \\sim N2 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma
of 0.03 and sigma for terminal atoms of 0.06
4. Rigid body (RIGU) restrains
 N1, C1B, N2B, C2B, C3B, C4B, C5B, C6B, C1, N2, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F1, F2, F3, F4, F5, F6, P1B, F1B, F2B, F3B, F4B, F5B, F6B, P7, F7, F8, F9,
  F10, F11, F12, P7B, F7B, F8B, F13, F14, F15, F16, P13, F17, F18, F19, F1A,
 F1C, F1D, P2, F1E, F1F, F1G, F1H, F1I, F1J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N101, C101, C102, N102, C103, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C1, N2, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1B, N2B, C2B, C3B, C4B, C5B, C6B}
{P1, F1, F2, F3, F4, F5, F6} sigma for 1-2: 0.01, 1-3: 0.04
as
{P1B, F1B, F2B, F3B, F4B, F5B, F6B}
{P7, F7, F8, F9, F10, F11, F12} sigma for 1-2: 0.01, 1-3: 0.04
as
{P7B, F7B, F8B, F13, F14, F15, F16}
{N101, C101, C102} sigma for 1-2: 0.01, 1-3: 0.04
as
{N102, C103, C104}
6. Others
 1*[Sof(C1)+Sof(H1A)+Sof(H1B)+Sof(N2)+Sof(C2)+Sof(C3)+Sof(H3)+Sof(C4)+Sof(H4)+
 Sof(C5)+Sof(H5)+Sof(C6)+Sof(H6)+Sof(C1B)+Sof(H1BA)+Sof(H1BB)+Sof(N2B)+Sof(C2B)+
 Sof(C3B)+Sof(H3B)+Sof(C4B)+Sof(H4B)+Sof(C5B)+Sof(H5B)+Sof(C6B)+Sof(H6B)+
 Sof(P7)+Sof(F7)+Sof(F8)+Sof(F9)+Sof(F10)+Sof(F11)+Sof(F12)]+1*[Sof(P7B)+
 Sof(F7B)+Sof(F8B)+Sof(F13)+Sof(F14)+Sof(F15)+Sof(F16)]=1 with esd of 0.0001
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(N2B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=
 Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(N2)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(P7)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=
 Sof(F11)=Sof(F12)=FVAR(1)
 Sof(P7B)=Sof(F7B)=Sof(F8B)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=FVAR(2)
 Sof(N102)=Sof(C103)=Sof(C104)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(3)
 Sof(N101)=Sof(C101)=Sof(C102)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
 Sof(P1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(4)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
 Sof(P2)=Sof(F1E)=Sof(F1F)=Sof(F1G)=Sof(F1H)=Sof(F1I)=Sof(F1J)=1-FVAR(5)
 Sof(P13)=Sof(F17)=Sof(F18)=Sof(F19)=Sof(F1A)=Sof(F1C)=Sof(F1D)=FVAR(5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1B(H1BA,H1BB), C7(H7A,H7B), C13(H13A,H13B), C19(H19A,H19B),
 C25(H25A,H25B), C31(H31A,H31B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B),
 C18(H18), C15(H15), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17),
 C019(H019), C29(H29), C28(H28), C27(H27), C24(H24), C23(H23), C22(H22),
 C21(H21), C35(H35), C34(H34), C33(H33), C30(H30)
7.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C104(H10D,H10E,H10F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'