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_7705716
_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         'C44 H54 Br2 Cl3 Dy O7 P2, 2(C2 H6 O)'
_chemical_formula_sum            'C48 H66 Br2 Cl3 Dy O9 P2'
_chemical_formula_weight         1277.61
_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                101.357(3)
_cell_angle_beta                 98.671(3)
_cell_angle_gamma                111.903(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2192(4)
_cell_length_b                   13.3757(4)
_cell_length_c                   20.6992(7)
_cell_measurement_reflns_used    57069
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.53
_cell_measurement_theta_min      3.71
_cell_volume                     2738.39(18)
_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 0.982
_diffrn_measured_fraction_theta_max 0.954
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20943
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.152
_diffrn_reflns_theta_min         3.706
_exptl_absorpt_coefficient_mu    11.311
_exptl_absorpt_correction_T_max  0.2375
_exptl_absorpt_correction_T_min  0.0380
_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    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0942P)^2^+3.2911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9981
_reflns_number_total             10129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           sv0796
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_original_cell_volume        2738.39(17)
_cod_database_code               7705716
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.200
_shelx_estimated_absorpt_t_min   0.150
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-C47
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C43A \\sim C44A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C43, C44, C43A, C44A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O7, C43, C44} sigma for 1-2: 0.02, 1-3: 0.04
{O7, C43A, C44A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7, C43, C44}
{O8, C45, C46} sigma for 1-2: 0.02, 1-3: 0.04
{O8, C45A, C46A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O8, C45, C46}
6. Others
 Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
 Sof(H8B)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46D)=Sof(H46E)=
 Sof(H46F)=1-FVAR(2)
 Sof(H8A)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C37(H37), C40(H40)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B), C43A(H43C,H43D), C45(H45A,H45B),
 C45A(H45C,H45D), C47(H47A,H47B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C25(H25), C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35)
7.d Tetrahedral OH refined with riding coordinates:
 O8(H8A), O8(H8B)
7.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C44(H44A,H44B,H44C), C44A(H44D,H44E,H44F), C46(H46A,H46B,H46C),
 C46A(H46D,H46E,H46F), C48(H48A,H48B,H48C)
7.f Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              94985
_shelx_fab_checksum              57511
_olex2_submission_special_instructions 'No special instructions were received'