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_7705721
_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
'C88 H108 Br4 Cl6 La2 O14 P4, C14 H8 Br2, 2(C2 H6 O)'
_chemical_formula_sum            'C106 H128 Br6 Cl6 La2 O16 P4'
_chemical_formula_weight         2751.94
_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   mixed
_audit_creation_date             2020-04-08
_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                97.274(3)
_cell_angle_beta                 98.726(3)
_cell_angle_gamma                93.626(3)
_cell_formula_units_Z            1
_cell_length_a                   13.4455(5)
_cell_length_b                   13.7347(6)
_cell_length_c                   15.6918(7)
_cell_measurement_reflns_used    24056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      1.33
_cell_volume                     2831.1(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.986
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22575
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.834
_diffrn_reflns_theta_min         1.326
_exptl_absorpt_coefficient_mu    3.120
_exptl_absorpt_correction_T_max  0.8398
_exptl_absorpt_correction_T_min  0.5808
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1378
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.050
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         11968
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0261P)^2^+9.8238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8675
_reflns_number_total             11968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           i2974
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_database_code               7705721
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H20D,H20E,H20F} of C20A, {H20A,H20B,H20C} of C20, {H42D,
  H42E,H42F} of C42A, {H53D,H53E,H53F} of C53A, {H42A,H42B,H42C} of C42, {H53A,
  H53B,H53C} of C53, All C(H,H) groups
 At 1.5 times of:
  {H21A,H21B,H21C} of C21, {H21D,H21E,H21F} of C21A, {H38A,H38B,H38C} of C38,
  {H39A,H39B,H39C} of C39, {H18A,H18B,H18C} of C18, {H17A,H17B,H17C} of C17,
  {H41D,H41E,H41F} of C41A, {H41A,H41B,H41C} of C41, {H44A,H44B,H44C} of C44
2. Uiso/Uaniso restraints and constraints
O3 \\sim C19 \\sim C20 \\sim C21: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O3A \\sim C19A \\sim C20A \\sim C21A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C40 \\sim C41 \\sim C42: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3. Rigid body (RIGU) restrains
 O3A, C19A, C20A, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{P1, O3A, C19A, C20A, C21A} sigma for 1-2: 0.02, 1-3: 0.04
as
{P1, O3, C19, C20, C21}
{O6, C40A, C41A, C42A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6, C40, C41, C42}
{O8, C52A, C53A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O8, C52, C53}
5. Others
 Sof(O3A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(O3)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=
 Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=FVAR(2)
 Sof(C52A)=Sof(H52C)=Sof(H52D)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(3)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C19A(H19A), C16(H16), C37(H37), C40(H40), C40A(H40A)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B), C52(H52A,H52B), C52A(H52C,H52D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7A), C12(H12), C11(H11), C13(H13), C14(H14),
 C25(H25), C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35),
  C48(H48), C49(H49), C50(H50), C51(H51)
6.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C20A(H20D,H20E,H20F), C21A(H21D,
 H21E,H21F), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C41A(H41D,H41E,
 H41F), C42A(H42D,H42E,H42F), C44(H44A,H44B,H44C), C53(H53A,H53B,H53C),
 C53A(H53D,H53E,H53F)
;
_shelx_res_checksum              76200
_olex2_submission_special_instructions 'No special instructions were received'