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_4348629
_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            'C92 H61 Cl12 N8 Nd'
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_space_group_name_Hall           '-P 2ybc'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.035(3)
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_cell_length_c                   30.201(6)
_cell_measurement_reflns_used    43340
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     8335(3)
_computing_cell_refinement       'Rigaku RAPID AUTO'
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_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
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_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku VariMax RAPID&#x0087;U'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'Rotating anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.4516
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3732
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         19093
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_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1144
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_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+11.5606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
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_reflns_number_total             19093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01442_si_002.cif
_cod_data_source_block           NdCHCl3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348629
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              93352
_shelx_hkl_checksum              49486