Lanthanide cryptate monometallic coordination complexes.
Buch, Christian D.; Mitcov, Dmitri; Piligkos, Stergios; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13557–13565; doi:10.1039/d0dt02448a

data_7705311
_publ_section_title
;
 Lanthanide cryptate monometallic coordination complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13557
_journal_page_last               13565
_journal_paper_doi               10.1039/d0dt02448a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C39 H45 N8 O3 Yb, 2(H2 O), H2 O1.5, 0.5(O)'
_chemical_formula_sum            'C39 H51 N8 O7 Yb'
_chemical_formula_weight         916.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-10 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.219(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2414(13)
_cell_length_b                   22.0413(19)
_cell_length_c                   27.359(3)
_cell_measurement_reflns_used    9069
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.558
_cell_measurement_theta_min      2.861
_cell_volume                     7984.9(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            126779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.328
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0878 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.8656. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             3736
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Slow evaporation of motherliqour'
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         11676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+29.5527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9854
_reflns_number_total             11676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02448a2.cif
_cod_data_source_block           d8v4166_0m
_cod_depositor_comments          'Adding full bibliography for 7705311.cif.'
_cod_original_cell_volume        7985.0(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7705311
_shelx_shelxl_version_number     2018/3
_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,H) groups
2. Others
 Sof(O0AB)=Sof(H0AC)=Sof(H0AD)=1-FVAR(1)
 Sof(O0AA)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
 Fixed Sof: H00F(0.5) H00G(0.5) H00H(0.5) H00I(0.5) O1AA(0.5) O1AB(0.5)
3.a Free rotating group:
 O008(H00F,H00G), O00Y(H00H,H00I), O0AA(H0AA,H0AB), O0AB(H0AC,H0AD), O1(H1A,H1B)
3.b Secondary CH2 refined with riding coordinates:
 C00R(H00A,H00B), C00V(H00C,H00D), C012(H01A,H01B), C013(H01C,H01D), C014(H01E,
 H01F), C017(H01G,H01H), C018(H01I,H01J), C01A(H01K,H01L), C01B(H01M,H01N),
 C01C(H01O,H01P), C01G(H01Z,H), C01H(H01,HA)
3.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00J(H00J), C00K(H00K), C00L(H00L), C00P(H00P), C00Q(H00Q),
 C00T(H00T), C00U(H00U), C00X(H00X), C010(H010), C015(H015), C016(H016)
3.d Idealised Me refined as rotating group:
 C01D(H01Q,H01R,H01S), C01E(H01T,H01U,H01V), C01F(H01W,H01X,H01Y)
;
_shelx_res_checksum              4760
_olex2_submission_special_instructions 'No special instructions were received'