Systematic Structural Elucidation for the Protonated Form of Rare Earth Bis(porphyrinato) Double-Decker Complexes: Direct Structural Evidence of the Location of the Attached Proton.
Yamashita, Ken-Ichi; Sakata, Naoya; Ogawa, Takuji; Inorganic chemistry 55 (2016) 8935–8942; doi:10.1021/acs.inorgchem.6b01442

data_4348631
_publ_section_title
;
 Systematic Structural Elucidation for the Protonated Form of Rare Earth
 Bis(porphyrinato) Double-Decker Complexes: Direct Structural Evidence of
 the Location of the Attached Proton.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8935
_journal_page_last               8942
_journal_paper_doi               10.1021/acs.inorgchem.6b01442
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C90 H61 Cl4 N8 Tb'
_chemical_formula_weight         1555.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.031(4)
_cell_length_b                   21.522(4)
_cell_length_c                   31.236(6)
_cell_measurement_reflns_used    34425
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     14138(5)
_computing_cell_refinement       'Rigaku RAPID AUTO'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku VariMax RAPID FR-E'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            33690
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Rotating anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7704
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             6320
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_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.714
_refine_diff_density_min         -2.712
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0887
_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^)+(0.0428P)^2^+472.0828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
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_reflns_number_total             4057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01442_si_002.cif
_cod_data_source_block           TbCH2Cl2
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4348631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.752
_shelx_res_checksum              74281
_shelx_hkl_checksum              31879