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_7040833
_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         'C36 H36 Mn2 N8 O2, C2 H3 N, 3(F6 P)'
_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                85.848(2)
_cell_angle_beta                 88.135(2)
_cell_angle_gamma                77.867(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6170(8)
_cell_length_b                   18.8980(12)
_cell_length_c                   19.9575(13)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.267
_cell_measurement_theta_min      2.209
_cell_volume                     4639.3(5)
_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      99.97
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            300185
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.250
_diffrn_reflns_theta_min         1.023
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0632 before and 0.0595 after correction. The Ratio of minimum to maximum transmission is 0.9674. 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    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         25833
_refine_ls_number_restraints     443
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0409P)^2^+5.3958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18009
_reflns_number_total             25833
_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               7040833
_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. Rigid body (RIGU) restrains
 P1A, F1A, F2A, F3A, F4A, F5A, F6A, P1B, F1B, F2B, F3B, F4B, F5B, F6B, P1C,
 F1C, F2C, F3C, F4C, F5C, F6C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P3A, F13A, F14A, F15A, F16A, F17A, F18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P3B, F13B, F14B, F15B, F16B, F17B, F18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Same fragment restrains
{P1A, F1A, F2A, F3A, F4A, F5A, F6A} sigma for 1-2: 0.01, 1-3: 0.04
as
{P1B, F1B, F2B, F3B, F4B, F5B, F6B}
{P1A, F1A, F2A, F3A, F4A, F5A, F6A} sigma for 1-2: 0.01, 1-3: 0.04
as
{P1C, F1C, F2C, F3C, F4C, F5C, F6C}
{P3A, F13A, F14A, F15A, F16A, F17A, F18A} sigma for 1-2: 0.01, 1-3: 0.04
as
{P3B, F13B, F14B, F15B, F16B, F17B, F18B}
{P3A, F13A, F14A, F15A, F16A, F17A, F18A} sigma for 1-2: 0.01, 1-3: 0.04
as
{P3C, F13C, F14C, F15C, F16C, F17C, F18C}
4. Others
 1*[Sof(P1A)+Sof(F1A)+Sof(F2A)+Sof(F3A)+Sof(F4A)+Sof(F5A)+Sof(F6A)]+1*
 [Sof(P1B)+Sof(F1B)+Sof(F2B)+Sof(F3B)+Sof(F4B)+Sof(F5B)+Sof(F6B)]+1*[Sof(P1C)+
 Sof(F1C)+Sof(F2C)+Sof(F3C)+Sof(F4C)+Sof(F5C)+Sof(F6C)]=1 with esd of 0.01
 1*[Sof(P3A)+Sof(F13A)+Sof(F14A)+Sof(F15A)+Sof(F16A)+Sof(F17A)+Sof(F18A)]+1*
 [Sof(P3B)+Sof(F13B)+Sof(F14B)+Sof(F15B)+Sof(F16B)+Sof(F17B)+Sof(F18B)]+1*
 [Sof(P3C)+Sof(F13C)+Sof(F14C)+Sof(F15C)+Sof(F16C)+Sof(F17C)+Sof(F18C)]=1 with
 esd of 0.01
 Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Sof(P1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=FVAR(2)
 Sof(P1C)=Sof(F1C)=Sof(F2C)=Sof(F3C)=Sof(F4C)=Sof(F5C)=Sof(F6C)=FVAR(3)
 Sof(P3A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=Sof(F18A)=FVAR(4)
 Sof(P3B)=Sof(F13B)=Sof(F14B)=Sof(F15B)=Sof(F16B)=Sof(F17B)=Sof(F18B)=FVAR(5)
 Sof(P3C)=Sof(F13C)=Sof(F14C)=Sof(F15C)=Sof(F16C)=Sof(F17C)=Sof(F18C)=FVAR(6)
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C7A(H7AA,H7AB), C7B(H7BA,H7BB), C13A(H13A,
 H13B), C13B(H13C,H13D), C19A(H19A,H19B), C19B(H19C,H19D), C25A(H25A,H25B),
 C25B(H25C,H25D), C31A(H31A,H31B), C31B(H31C,H31D)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C9A(H9A), C9B(H9B), C10A(H10A),
 C10B(H10B), C11A(H11A), C11B(H11B), C12A(H12A), C12B(H12B), C15A(H15A),
 C15B(H15B), C16A(H16A), C16B(H16B), C17A(H17A), C17B(H17B), C18A(H18A),
 C18B(H18B), C21A(H21A), C21B(H21B), C22A(H22A), C22B(H22B), C23A(H23A),
 C23B(H23B), C24A(H24A), C24B(H24B), C27A(H27A), C27B(H27B), C28A(H28A),
 C28B(H28B), C29A(H29A), C29B(H29B), C30A(H30A), C30B(H30B), C33A(H33A),
 C33B(H33B), C34A(H34A), C34B(H34B), C35A(H35A), C35B(H35B), C36A(H36A),
 C36B(H36B), C3B1(H3B1), C4B1(H4B1), C5B1(H5B1), C6B1(H6B1)
5.c Idealised Me refined as rotating group:
 C102(H10C,H10D,H10E), C93(H93A,H93B,H93C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'