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_7703283
_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 Ho N5 O8 P, Ca0.5, 6(H2 O)'
_chemical_formula_sum            'C30 H52 Ca0.5 Ho N5 O14 P'
_chemical_formula_weight         922.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 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                90
_cell_angle_beta                 95.775(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.1798(13)
_cell_length_b                   10.1265(5)
_cell_length_c                   15.2799(8)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.3718
_cell_measurement_theta_min      2.4166
_cell_volume                     3722.4(3)
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56881
_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         27.549
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'I\mS micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.309
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.79
_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    1.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.026
_refine_diff_density_max         5.593
_refine_diff_density_min         -9.245
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8553
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.337
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.1022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+139.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7679
_reflns_number_total             8553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04056k2.cif
_cod_data_source_block           hodbamoh
_cod_depositor_comments
'Adding full bibliography for 7703270--7703283.cif.'
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C30 H52 Ca0.50 Ho N5 O14 P'
_cod_database_code               7703283
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              3964