Imposing high-symmetry and tuneable geometry on lanthanide centres with chelating Pt and Pd metalloligands
Sørensen, Mikkel A.; Weihe, Høgni; Vinum, Morten G.; Mortensen, Jesper S.; Doerrer, Linda H.; Bendix, Jesper; Chem. Sci. 8 (2017) 3566–; doi:10.1039/C7SC00135E

data_1545354
_publ_section_title
;
 Imposing high-symmetry and tuneable geometry on lanthanide centres with
 chelating Pt and Pd metalloligands
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3566
_journal_paper_doi               10.1039/C7SC00135E
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C16 H24 Gd O8 Pd2 S8, C8 H20 N'
_chemical_formula_sum            'C24 H44 Gd N O8 Pd2 S8'
_chemical_formula_weight         1101.23
_space_group_crystal_system      tetragonal
_space_group_IT_number           124
_space_group_name_Hall           '-P 4 2c'
_space_group_name_H-M_alt        'P 4/m c c'
_symmetry_Int_Tables_number      124
_symmetry_space_group_name_Hall  '-P 4 2c'
_symmetry_space_group_name_H-M   'P 4/m c c'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-01-09 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6832(2)
_cell_length_b                   8.6832(2)
_cell_length_c                   25.8856(9)
_cell_measurement_reflns_used    7198
_cell_measurement_temperature    295
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.35
_cell_volume                     1951.72(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32169
_diffrn_reflns_theta_full        27.4685
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.060
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0679 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.8778.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.8737
_exptl_crystal_description       plate
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.7560
_refine_diff_density_min         -0.9857
_refine_diff_density_rms         0.2183
_refine_ls_d_res_high            0.7704
_refine_ls_d_res_low             8.6832
_refine_ls_goodness_of_fit_ref   1.1018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1160
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.1003
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+2.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                863
_reflns_number_total             1160
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7sc00135e2.cif
_cod_data_source_block           1Gd-Pd-RT
_cod_depositor_comments
'Adding full bibliography for 1545338--1545364.cif.'
_cod_database_code               1545354
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-H4b
 0.96 with sigma of 0.02
 C4-H4a
 0.96 with sigma of 0.02
 C4-H4c
 0.96 with sigma of 0.02
3. Others
 Fixed Sof: S1(0.5) O1(0.5) C3(0.5) S1a(0.5) O1a(0.5) H4a(0.37) H4b(0.475)
 H4c(0.655)
4.a Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'