The solid-state structures and ligand cavity evaluation of lanthanide(iii) complexes of a DOTA analogue with a (dibenzylamino)methylphosphinate pendant arm.
Urbanovský, Peter; Kotek, Jan; Císařová, Ivana; Hermann, Petr; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1555–1569; doi:10.1039/c9dt04056k

data_7703276
_publ_section_title
;
 The solid-state structures and ligand cavity evaluation of
 lanthanide(iii) complexes of a DOTA analogue with a
 (dibenzylamino)methylphosphinate pendant arm.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1555
_journal_page_last               1569
_journal_paper_doi               10.1039/c9dt04056k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C60 H92 N10 Na2 O22 P2 Yb2, 6(H2 O)'
_chemical_formula_sum            'C60 H104 N10 Na2 O28 P2 Yb2'
_chemical_formula_weight         1867.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.544(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   49.3984(12)
_cell_length_b                   10.1801(2)
_cell_length_c                   15.3464(4)
_cell_measurement_reflns_used    9229
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.0154
_cell_measurement_theta_min      2.4038
_cell_volume                     7533.2(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2014.11.0.1'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.689
_exptl_absorpt_coefficient_mu    2.608
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7410
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+77.5617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6343
_reflns_number_total             7410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04056k2.cif
_cod_data_source_block           dbam_yb
_cod_depositor_comments
;
Adding full bibliography for 7703270--7703283.cif.

2024-04-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H52 N5 Na O14 P Yb'
_cod_original_formula_weight         933.76
_cod_original_formula_moiety         'C30 H40 N5 O8 P Yb, Na, 6(H2 O)'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7703276
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.389
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              35046