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_7040830
_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         'C21 H18 Mn N4 O3, 0.99(F6 P)'
_chemical_formula_sum            'C21 H18 F5.97 Mn N4 O3 P0.99'
_chemical_formula_weight         573.52
_chemical_name_common            Mn(tpa)(CO)3(PF6)
_chemical_name_systematic
tris(2-pyridylmethyl)amine-tris(carbonyl)manganese(hexafluorophosphate)
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 100.432(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9782(7)
_cell_length_b                   13.3015(9)
_cell_length_c                   15.8036(11)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.97
_cell_measurement_theta_min      2.43
_cell_volume                     2269.6(3)
_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      100.09
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.886
_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  0.0227
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37391
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.408
_diffrn_reflns_theta_min         2.015
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.7141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0507 before and 0.0382 after correction. The Ratio of minimum to maximum transmission is 0.9565. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             1159
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0384P)^2^+1.0247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6405
_reflns_number_total             7822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02020h3.cif
_cod_data_source_block           p21n_a
_cod_depositor_comments
'Adding full bibliography for 7040830--7040834.cif.'
_cod_database_code               7040830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 P91A, F91A, F93A, F92A, F94A, F95A, F96A, P91B, F91B, F93B, F92B, F94B, F95B,
 F96B, P91C, F91C, F93C, F92C, F94C, F95C, F96C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Same fragment restrains
{P91A, F91A, F93A, F92A, F94A, F95A, F96A, P91B, F91B, F93B, F92B, F94B, F95B,
F96B} sigma for 1-2: 0.01, 1-3: 0.04
{P91A, F91A, F93A, F92A, F94A, F95A, F96A, P91C, F91C, F93C, F92C, F94C, F95C,
F96C} sigma for 1-2: 0.01, 1-3: 0.04
as
{P91A, F91A, F93A, F92A, F94A, F95A, F96A, P91B, F91B, F93B, F92B, F94B, F95B,
F96B}
4. Others
 1*[Sof(P91B)+Sof(F91B)+Sof(F93B)+Sof(F92B)+Sof(F94B)+Sof(F95B)+Sof(F96B)]+1*
 [Sof(P91A)+Sof(F91A)+Sof(F93A)+Sof(F92A)+Sof(F94A)+Sof(F95A)+Sof(F96A)]+1*
 [Sof(P91C)+Sof(F91C)+Sof(F93C)+Sof(F92C)+Sof(F94C)+Sof(F95C)+Sof(F96C)]=1 with
 esd of 0.01
 Sof(P91B)=Sof(F91B)=Sof(F93B)=Sof(F92B)=Sof(F94B)=Sof(F95B)=Sof(F96B)=FVAR(1)
 Sof(P91A)=Sof(F91A)=Sof(F93A)=Sof(F92A)=Sof(F94A)=Sof(F95A)=Sof(F96A)=FVAR(2)
 Sof(P91C)=Sof(F91C)=Sof(F93C)=Sof(F92C)=Sof(F94C)=Sof(F95C)=Sof(F96C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'