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_7705718
_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         'C63 H74 Br3 Cl3 Nd O10 P3'
_chemical_formula_sum            'C63 H74 Br3 Cl3 Nd O10 P3'
_chemical_formula_weight         1574.45
_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                103.591(4)
_cell_angle_beta                 100.785(4)
_cell_angle_gamma                111.726(4)
_cell_formula_units_Z            2
_cell_length_a                   13.6169(7)
_cell_length_b                   15.8635(9)
_cell_length_c                   17.6449(8)
_cell_measurement_reflns_used    21648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      1.25
_cell_volume                     3279.2(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 0.995
_diffrn_measured_fraction_theta_max 0.981
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26012
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.851
_diffrn_reflns_theta_min         1.246
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  0.9357
_exptl_absorpt_correction_T_min  0.4904
_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    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         13831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0360P)^2^+12.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9355
_reflns_number_total             13831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           i2983
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_database_code               7705718
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.558
_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. Same fragment restrains
{O10, H10A, H10B} sigma for 1-2: 0.02, 1-3: 0.04
as
{Nd1, C1, Br1}
3.a Ternary CH refined with riding coordinates:
 C19(H19), C16(H16), C40(H40), C37(H37), C58(H58), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C25(H25), C26(H26), C32(H32), C33(H33), C27(H27), C28(H28), C34(H34), C35(H35),
  C53(H53), C54(H54), C55(H55), C56(H56), C49(H49), C48(H48), C47(H47), C46(H46)
3.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              60385
_olex2_submission_special_instructions 'No special instructions were received'