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_7040832
_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         'C32 H28 Mn2 N16 O8, 8(H2 O)'
_chemical_formula_sum            'C32 H44 Mn2 N16 O16'
_chemical_formula_weight         1018.71
_chemical_name_common
tetra(bispyrazolylaceticacid)bis(manganese(II))tetra(hexafluorophosphate)
_chemical_name_systematic
tetra(bispyrazolylaceticacid)bis(manganese(II))tetra(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   mixed
_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                103.770(4)
_cell_angle_beta                 95.537(4)
_cell_angle_gamma                94.757(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3617(10)
_cell_length_b                   10.9758(10)
_cell_length_c                   12.1705(12)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.147
_cell_measurement_theta_min      2.462
_cell_volume                     1073.30(19)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.864
_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  0.0188
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.697
_diffrn_reflns_theta_min         1.735
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.7019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0720 before and 0.0317 after correction. The Ratio of minimum to maximum transmission is 0.9394. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         9236
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0381P)^2^+0.4092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8312
_reflns_number_total             9236
_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               7040832
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O101-H10A = O101-H10B = O103-H10C = O103-H10D = O105-H10E = O105-H10F
 0.9584 with sigma of 0.01
 O107-H10H = O107-H10G
 0.9584 with sigma of 0.01
 H10A-H10B = H10C-H10D = H10E-H10F = H10H-H10G
 1.5151 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C1(H1), C9(H9)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C5(H5), C8(H8), C7(H7), C16(H16), C15(H15), C14(H14),
 C13(H13), C12(H12), C11(H11)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'