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_7703274
_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         'C30 H40 Er N5 O8 P, Na, 4.25(H2 O)'
_chemical_formula_sum            'C30 H48.5 Er N5 Na O12.25 P'
_chemical_formula_weight         896.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                77.957(3)
_cell_angle_beta                 78.577(3)
_cell_angle_gamma                89.761(3)
_cell_formula_units_Z            4
_cell_length_a                   10.2212(10)
_cell_length_b                   15.3230(13)
_cell_length_c                   25.162(2)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9871
_cell_measurement_theta_min      2.4030
_cell_volume                     3774.9(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.987
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.360
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             1822
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.179
_refine_diff_density_max         7.077
_refine_diff_density_min         -5.420
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         14762
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0915
_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^)+(0.0001P)^2^+149.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13327
_reflns_number_total             14762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04056k2.cif
_cod_data_source_block           er_do3apdbam
_cod_depositor_comments
'Adding full bibliography for 7703270--7703283.cif.'
_cod_original_formula_sum        'C30 H48.50 Er N5 Na O12.25 P'
_cod_database_code               7703274
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.448
_shelx_estimated_absorpt_t_max   0.679
_shelx_res_checksum              1468