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_4347443
_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
'C57 H52 Mn N5, C18 H36 K N2 O6, 1.629(C6 H5 Cl)'
_chemical_formula_sum            'C84.77 H96.15 Cl1.63 K Mn N7 O6'
_chemical_formula_weight         1461.05
_chemical_name_common            '[K(222)][Mn(TMP)(CN)]1.63(C6H5Cl)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2231(6)
_cell_length_b                   24.3062(12)
_cell_length_c                   24.7602(13)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.1816
_cell_measurement_theta_min      2.2535
_cell_volume                     7958.0(7)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2014; Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXP-2014/6 (Sheldrick, 2014)'
_computing_publication_material
'SHELXCIF (Sheldrick, 2014)/enCIFer (CCDC, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Brucker D8 QUEST System'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            139376
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.128
_diffrn_reflns_theta_min         2.254
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2008) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3094
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         17528
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0833P)^2^+6.0580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                16196
_reflns_number_total             17528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00173_si_002.cif
_cod_data_source_block           20150124_MnTMPCN_K222
_cod_database_code               4347443
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.949
_shelxl_version_number           2014/6
_shelx_res_checksum              25518
_shelx_hkl_checksum              20414