Determination of the Structural Parameters of Heteronuclear (Phthalocyaninato)bis(crownphthalocyaninato)lanthanide(III) Triple-Deckers in Solution by Simultaneous Analysis of NMR and Single-Crystal X-ray Data.
Polovkova, Marina A.; Martynov, Alexander G.; Birin, Kirill P.; Nefedov, Sergey E.; Gorbunova, Yulia G.; Tsivadze, Aslan Yu; Inorganic chemistry 55 (2016) 9258–9269; doi:10.1021/acs.inorgchem.6b01292

data_4348524
_publ_section_title
;
 Determination of the Structural Parameters of Heteronuclear
 (Phthalocyaninato)bis(crownphthalocyaninato)lanthanide(III)
 Triple-Deckers in Solution by Simultaneous Analysis of NMR and
 Single-Crystal X-ray Data.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9258
_journal_page_last               9269
_journal_paper_doi               10.1021/acs.inorgchem.6b01292
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C164 H170 Cl12 N24 O43 Y Yb'
_chemical_formula_weight         3852.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.097(2)
_cell_length_b                   35.554(3)
_cell_length_c                   45.696(3)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.09
_cell_measurement_theta_min      2.22
_cell_volume                     47273(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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_unetI/netI     0.2822
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40811
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.863
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       prizm
_exptl_crystal_F_000             15832
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.778
_refine_diff_density_min         -2.258
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         40811
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.2181
_refine_ls_R_factor_gt           0.1084
_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^)+(0.1882P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2723
_refine_ls_wR_factor_ref         0.3145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14410
_reflns_number_total             40811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01292_si_003.cif
_cod_data_source_block           yby
_cod_original_cell_volume        47274(6)
_cod_database_code               4348524
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.825
_shelx_estimated_absorpt_t_max   0.851
_shelx_res_checksum              16086
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_shelx_fab_checksum              1886