Functionalised phosphonate ester supported lanthanide (Ln = La, Nd, Dy, Er) complexes.
Koehne, Ingo; Lik, Artur; Gerstel, Miriam; Bruhn, Clemens; Reithmaier, Johann Peter; Benyoucef, Mohamed; Pietschnig, Rudolf; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16683–16692; doi:10.1039/d0dt03047c

data_7705712
_publ_section_title
;
 Functionalised phosphonate ester supported lanthanide (Ln = La, Nd, Dy,
 Er) complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16683
_journal_page_last               16692
_journal_paper_doi               10.1039/d0dt03047c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C39 H63 Dy N3 O18 P3'
_chemical_formula_sum            'C39 H63 Dy N3 O18 P3'
_chemical_formula_weight         1117.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.899(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0470(5)
_cell_length_b                   21.2523(7)
_cell_length_c                   16.3650(6)
_cell_measurement_reflns_used    44766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      1.26
_cell_volume                     5183.6(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.71.4.0 (STOE, 2017)
;
_computing_molecular_graphics    'Mercury (P. A. Wood et al., 2020)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
 201 frames, detector distance = 110 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2, 0.6 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.719
_diffrn_reflns_theta_min         1.580
_diffrn_source                   'Genix Mo HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         9767
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+3.5567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8484
_reflns_number_total             9767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           i2894
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_database_code               7705712
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O6A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38A, C38, C39, C39A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
 C37A, C37, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
3. Same fragment restrains
{O6A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6, C24, C25, C26}
{O9, C37A, C38A, C39A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O9, C37, C38, C39}
{O5, C21A, C22A, C23A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5, C21, C22, C23}
4. Others
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(2)
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=FVAR(2)
 Sof(O6A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(3)
 Sof(O6)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C24(H24), C24A(H24A), C34(H34), C37(H37), C37A(H37A),
 C21(H21), C21A(H21A)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B), C27(H27A,H27B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C20(H20), C19(H19), C18(H18),
 C17(H17), C16(H16), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
5.d Fitted hexagon refined as free rotating group:
 C15(C20,C19,C18,C17,C16)
5.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C38A(H38D,H38E,H38F), C39A(H39D,H39E,H39F),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C22A(H22D,H22E,H22F), C23A(H23D,H23E,
 H23F)
;
_shelx_res_checksum              36206
_olex2_submission_special_instructions 'No special instructions were received'