Axial Mn-CCN Bonds of Cyano Manganese(II) Porphyrin Complexes: Flexible and Weak?
He, Mingrui; Li, Xiangjun; Liu, Yanhong; Li, Jianfeng; Inorganic chemistry 55 (2016) 5871–5879; doi:10.1021/acs.inorgchem.6b00173

data_4347445
_publ_section_title
;
 Axial Mn-CCN Bonds of Cyano Manganese(II) Porphyrin Complexes: Flexible
 and Weak?
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5871
_journal_page_last               5879
_journal_paper_doi               10.1021/acs.inorgchem.6b00173
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C49 H36 Mn N5, C18 H36 K N2 O6, C6 H5 Cl'
_chemical_formula_sum            'C73 H77 Cl K Mn N7 O6'
_chemical_formula_weight         1277.90
_chemical_name_common            '[K(222)][Mn(TTP)(CN)]PhCl'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                81.690(2)
_cell_angle_beta                 74.862(2)
_cell_angle_gamma                86.134(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7796(3)
_cell_length_b                   14.8337(4)
_cell_length_c                   20.0496(6)
_cell_measurement_reflns_used    11742
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1724
_cell_measurement_theta_min      3.0948
_cell_volume                     3344.68(16)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.35.19'
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.35.19'
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.35.19'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material
'SHELXCIF-2014/6 (Sheldrick, 2014)/enCEFer(CCDC, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2141
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40103
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.101
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1346
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.433
_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     802
_refine_ls_number_reflns         13139
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+3.8386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10371
_reflns_number_total             13139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00173_si_005.cif
_cod_data_source_block           20140327_MnTTPCN_K222
_cod_database_code               4347445
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.900
_shelxl_version_number           2014/6
_shelx_res_checksum              47007
_shelx_hkl_checksum              52004