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_7705710
_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 N3 Nd O18 P3'
_chemical_formula_sum            'C39 H63 N3 Nd O18 P3'
_chemical_formula_weight         1099.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 97.312(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3724(7)
_cell_length_b                   20.4341(6)
_cell_length_c                   16.3173(6)
_cell_measurement_reflns_used    47708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      1.34
_cell_volume                     5083.9(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      100.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35429
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.720
_diffrn_reflns_theta_min         1.258
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.9178
_exptl_absorpt_correction_T_min  0.3265
_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    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.585
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 6647 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         19054
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+6.8169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                16024
_reflns_number_total             19054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           i2902
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_database_code               7705710
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H48A,H48B,H48C} of C48, All C(H,H) groups
 At 1.5 times of:
  {H35A,H35B,H35C} of C35, {H77A,H77B,H77C} of C77, {H75A,H75B,H75C} of C75,
  {H38A,H38B,H38C} of C38, {H36A,H36B,H36C} of C36, {H78A,H78B,H78C} of C78,
  {H74A,H74B,H74C} of C74, {H39A,H39B,H39C} of C39, {H13D,H13E,H13F} of C13A,
  {H9A,H9B,H9C} of C9, {H10A,H10B,H10C} of C10, {H9AA,H9AB,H9AC} of C9A, {H10D,
  H10E,H10F} of C10A, {H12A,H12B,H12C} of C12, {H13A,H13B,H13C} of C13, {H12D,
  H12E,H12F} of C12A, {H49D,H49E,H49F} of C49A, {H49A,H49B,H49C} of C49, {H48D,
  H48E,H48F} of C48A, {H65A,H65B,H65C} of C65, {H64A,H64B,H64C} of C64, {H25A,
  H25B,H25C} of C25, {H51A,H51B,H51C} of C51, {H61A,H61B,H61C} of C61, {H26A,
  H26B,H26C} of C26, {H62A,H62B,H62C} of C62, {H52A,H52B,H52C} of C52, {H23A,
  H23B,H23C} of C23, {H22A,H22B,H22C} of C22
2. Uiso/Uaniso restraints and constraints
O2 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O2A \\sim C8A \\sim C9A \\sim C10A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O3 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O3A \\sim C11A \\sim C12A \\sim C13A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O20 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O20A \\sim C47A \\sim C48A \\sim C49A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C49) = Uanis(C49A)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
3. Rigid body (RIGU) restrains
 C9, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O20A, C47A, C48A, C49A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C28, C29, C30, C31, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C10A, C9, C9A, C8A, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
4. Same fragment restrains
{P2, O5, C21, C22, C23} sigma for 1-2: 0.02, 1-3: 0.04
{P1, O2A, C8A, C9A, C10A} sigma for 1-2: 0.02, 1-3: 0.04
as
{P1, O2, C8, C9, C10}
{O3A, C11A, C12A, C13A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3, C11, C12, C13}
{P4, O20A, C47A, C48A, C49A} sigma for 1-2: 0.02, 1-3: 0.04
as
{P4, O20, C47, C48, C49}
{P3, C27A, C28A, C29A, C30A, C31A, C32A, C33A} sigma for 1-2: 0.02, 1-3: 0.04
as
{P3, C27, C28, C29, C30, C31, C32, C33}
5. Others
 Sof(O2A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(O2)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(O3A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(2)
 Sof(O3)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(2)
 Sof(O20A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=
 Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(3)
 Sof(O20)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(3)
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=
 Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=1-FVAR(4)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=
 Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C8A(H8A), C11(H11), C11A(H11A), C47(H47), C47A(H47A), C21(H21),
 C24(H24), C50(H50), C60(H60), C63(H63), C73(H73), C76(H76), C34(H34), C37(H37)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B), C40(H40A,H40B), C53(H53A,H53B), C66(H66A,H66B),
 C27(H27A,H27B), C27A(H27C,H27D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C6(H6), C20(H20), C16(H16), C18(H18), C17(H17),
 C19(H19), C42(H42), C43(H43), C46(H46), C45(H45), C44(H44), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59), C68(H68), C69(H69), C70(H70), C71(H71),
 C72(H72), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C29A(H29A),
 C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C3(H3)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,
 H10F), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C12A(H12D,H12E,H12F),
 C13A(H13D,H13E,H13F), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C48A(H48D,H48E,
 H48F), C49A(H49D,H49E,H49F), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), 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), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C75(H75A,H75B,H75C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              98881
_olex2_submission_special_instructions 'No special instructions were received'