Heteroleptic, polynuclear dysprosium(iii)-carbamato complexes through in situ carbon dioxide capture.
Schlittenhardt, Sören; Moreno-Pineda, Eufemio; Ruben, Mario; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4735–4742; doi:10.1039/d1dt00063b

data_7706862
_publ_section_title
;
 Heteroleptic, polynuclear dysprosium(iii)-carbamato complexes through in
 situ carbon dioxide capture.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4735
_journal_page_last               4742
_journal_paper_doi               10.1039/d1dt00063b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C76 H154 Dy4 N10 O24, C7 H8'
_chemical_formula_sum            'C83 H162 Dy4 N10 O24'
_chemical_formula_weight         2334.22
_chemical_properties_physical    Moisture-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-10 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0169(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3429(3)
_cell_length_b                   16.74118(16)
_cell_length_c                   25.2476(3)
_cell_measurement_reflns_used    25772
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      27.0790
_cell_measurement_theta_min      2.1050
_cell_volume                     10477.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_detector                 'imaging plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -90.00  80.00   1.00  240.60    --    0.00 180.00 214.00  170
  2  \w    -90.00 -30.00   1.00  240.60    --    0.00 180.00  32.00   60
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0191398000
_diffrn_orient_matrix_UB_12      -0.0041218000
_diffrn_orient_matrix_UB_13      -0.0167112000
_diffrn_orient_matrix_UB_21      0.0188612000
_diffrn_orient_matrix_UB_22      0.0227047000
_diffrn_orient_matrix_UB_23      0.0187484000
_diffrn_orient_matrix_UB_31      0.0098467000
_diffrn_orient_matrix_UB_32      -0.0355371000
_diffrn_orient_matrix_UB_33      0.0139213000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48544
_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         26.372
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             4744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+4.3518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9201
_reflns_number_total             10687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00063b2.cif
_cod_data_source_block           sor-8_1
_cod_depositor_comments
'Adding full bibliography for 7706862--7706864.cif.'
_cod_original_cell_volume        10477.09(18)
_cod_database_code               7706862
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Dy4 N10 O24 C76 H154'
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.655
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Restrained distances
 C105-C107 \\sim C107-C101
 with sigma of 0.02
 N4B-C4 \\sim C4-N4A
 with sigma of 0.02
 C27B-N4B \\sim N4B-C24B \\sim C27A-N4A \\sim N4A-C24A
 with sigma of 0.02
 C25B-C24B \\sim C24B-C26B \\sim C26A-C24A \\sim C24A-C25A \\sim C28A-C27A
\\sim C27A-C29A \\sim C29B-
 C27B \\sim C27B-C28B
 with sigma of 0.02
3. Restrained planarity
 C105, C101, C102, C106, C103, C107, C104
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 N4A, C29A, C26A, C27A, C25A, C24A, C28A, C4
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 N4B, C24B, C27B, C25B, C26B, C28B, C29B, C4
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 C105, C107, C106, C101, C102, C104, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N4B)=Sof(C24B)=Sof(H24B)=Sof(C27B)=Sof(H27B)=Sof(C25B)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C28B)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(N4A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C26A)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C27A)=Sof(H27A)=Sof(C25A)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C24A)=Sof(H24A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Fixed Sof: C107(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C106(0.5) C101(0.5)
 H101(0.5) C102(0.5) H102(0.5) C103(0.5) H103(0.5) C104(0.5) H104(0.5)
 C105(0.5) H105(0.5)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C30(H30), C9(H9), C33(H33), C21(H21), C18(H18), C6(H6),
 C27A(H27A), C24A(H24A), C24B(H24B), C27B(H27B)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C36(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C101(H101), C102(H102), C103(H103), C104(H104), C105(H105)
6.d Fitted hexagon refined as free rotating group:
 C106(C101,C102,C103,C104,C105)
6.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C38(H38A,H38B,H38C), C13(H13A,H13B,H13C), C11(H11A,H11B,
 H11C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C16(H16A,H16B,H16C), C14(H14A,
 H14B,H14C), C34(H34A,H34B,H34C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C),
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C35(H35A,H35B,H35C),
  C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C29A(H29A,H29B,H29C), C26A(H26A,H26B,
 H26C), C25A(H25A,H25B,H25C), C28A(H28A,H28B,H28C), C25B(H25D,H25E,H25F),
 C26B(H26D,H26E,H26F), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C107(H10D,
 H10E,H10F)
;
_shelx_res_checksum              23994
_shelx_hkl_checksum              62933
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.118
_oxdiff_exptl_absorpt_empirical_full_min 0.917