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_7703270
_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 H41 Ce N5 O8 P, 0.5(H4 N), 6.5(H2 O), Cl0.5'
_chemical_formula_sum            'C30 H56 Ce Cl0.5 N5.5 O14.5 P'
_chemical_formula_weight         914.61
_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   mixed
_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                68.256(2)
_cell_angle_beta                 79.612(2)
_cell_angle_gamma                78.900(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7568(8)
_cell_length_b                   12.4231(9)
_cell_length_c                   14.5497(10)
_cell_measurement_reflns_used    9024
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5189
_cell_measurement_theta_min      2.4722
_cell_volume                     1923.0(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v6.2.9'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         2.338
_diffrn_source                   'I\mS micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       bar
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.899
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0340P)^2^+4.0147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8293
_reflns_number_total             8828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04056k2.cif
_cod_data_source_block           cedbamh
_cod_depositor_comments
'Adding full bibliography for 7703270--7703283.cif.'
_cod_original_formula_sum        'C30 H56 Ce Cl0.50 N5.50 O14.50 P'
_cod_database_code               7703270
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              75459