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_7703279
_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 H42 N5 O9 P Sm, 3(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 N6 O12 P Sm'
_chemical_formula_weight         870.09
_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   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                 90.6500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.041(8)
_cell_length_b                   10.2877(14)
_cell_length_c                   15.205(2)
_cell_measurement_reflns_used    9270
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5592
_cell_measurement_theta_min      2.4258
_cell_volume                     7357.9(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
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_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 0.998
_diffrn_measured_fraction_theta_max 0.970
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       13
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_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            102754
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.040
_diffrn_reflns_theta_min         2.368
_diffrn_source                   'I\mS micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.46
_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    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.131
_refine_diff_density_max         3.990
_refine_diff_density_min         -6.087
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8668
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.463
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0626
_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^)+252.6453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8435
_reflns_number_total             8668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04056k2.cif
_cod_data_source_block           smdbamoh
_cod_depositor_comments
'Adding full bibliography for 7703270--7703283.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7703279
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              51229