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_7705714
_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         '0.5(C78 H120 Br6 N6 Nd2 O36 P6)'
_chemical_formula_sum            'C39 H60 Br3 N3 Nd O18 P3'
_chemical_formula_weight         1335.78
_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_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                61.9330(10)
_cell_angle_beta                 70.4940(10)
_cell_angle_gamma                67.9000(10)
_cell_formula_units_Z            4
_cell_length_a                   16.4380(3)
_cell_length_b                   20.2226(3)
_cell_length_c                   20.3926(3)
_cell_measurement_reflns_used    120459
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.21
_cell_measurement_theta_min      2.51
_cell_volume                     5439.19(16)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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 1.83, Darmstadt 2018
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61374
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.474
_diffrn_reflns_theta_min         2.502
_exptl_absorpt_coefficient_mu    11.279
_exptl_absorpt_correction_T_max  0.2169
_exptl_absorpt_correction_T_min  0.0426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
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    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.179
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         19710
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+7.2803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18960
_reflns_number_total             19710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           sv0709
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_original_cell_volume        5439.20(16)
_cod_database_code               7705714
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.237
_shelx_estimated_absorpt_t_min   0.095
_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. Uiso/Uaniso restraints and constraints
O11 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O11A \\sim C8A \\sim C9A \\sim C10A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O36 \\sim C76 \\sim C77 \\sim C78: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O36A \\sim C76A \\sim C77A \\sim C78A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 O11A, C8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O36A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{P1, O11A, C8A, C9A, C10A} sigma for 1-2: 0.02, 1-3: 0.04
as
{P1, O11, C8, C9, C10}
{P6, O36A, C76A, C77A, C78A} sigma for 1-2: 0.02, 1-3: 0.04
as
{P6, O36, C76, C77, C78}
5. Others
 Sof(O11A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(O11)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(O36A)=Sof(C76A)=Sof(H76A)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=
 Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(2)
 Sof(O36)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=
 Sof(H78A)=Sof(H78B)=Sof(H78C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C24(H24), C34(H34), C37(H37), C47(H47), C50(H50),
 C60(H60), C63(H63), C73(H73), C8(H8), C8A(H8A), C76(H76), C76A(H76A)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C20(H20A,H20B), C33(H33A,H33B), C46(H46A,H46B), C59(H59A,H59B),
 C72(H72A,H72B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C14(H14), C15(H15), C17(H17), C18(H18),
 C27(H27), C28(H28), C30(H30), C31(H31), C40(H40), C41(H41), C43(H43), C44(H44),
  C53(H53), C54(H54), C56(H56), C57(H57), C66(H66), C67(H67), C69(H69), C70(H70)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C74(H74A,
 H74B,H74C), C75(H75A,H75B,H75C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C77A(H77D,H77E,H77F), C78A(H78D,H78E,H78F)
;
_shelx_res_checksum              83320
_olex2_submission_special_instructions 'No special instructions were received'