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_7705720
_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 H72 Br3 Cl3 Er O9 P3, C4 H8 O'
_chemical_formula_sum            'C67 H80 Br3 Cl3 Er O10 P3'
_chemical_formula_weight         1651.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 115.243(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3578(6)
_cell_length_b                   16.3493(6)
_cell_length_c                   22.3921(6)
_cell_measurement_reflns_used    44914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.82
_cell_measurement_theta_min      2.29
_cell_volume                     7072.3(4)
_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 0.976
_diffrn_measured_fraction_theta_max 0.965
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26810
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.984
_diffrn_reflns_theta_min         2.287
_exptl_absorpt_coefficient_mu    6.311
_exptl_absorpt_correction_T_max  0.7427
_exptl_absorpt_correction_T_min  0.1046
_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    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.054
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         12928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1328P)^2^+11.9508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10927
_reflns_number_total             12928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           sv0773
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_database_code               7705720
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H39A,H39B,H39C} of C39, All C(H,H) groups
 At 1.5 times of:
  {H20A,H20B,H20C} of C20, {H18A,H18B,H18C} of C18, {H17A,H17B,H17C} of C17,
  {H21A,H21B,H21C} of C21, {H38A,H38B,H38C} of C38, {H59A,H59B,H59C} of C59,
  {H60A,H60B,H60C} of C60, {H62A,H62B,H62C} of C62, {H63A,H63B,H63C} of C63,
  {H42A,H42B,H42C} of C42, {H41A,H41B,H41C} of C41
2.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C37(H37), C40(H40), C58(H58), C61(H61)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B)
2.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), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35),
  C46(H46), C47(H47), C48(H48), C49(H49), C53(H53), C54(H54), C55(H55), C56(H56)
2.d 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), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C)
;
_shelx_res_checksum              80260
_olex2_submission_special_instructions 'No special instructions were received'