Crystal structure of dipyridine-k1 N-tris(2,2,6,6-tetramethyl-5-oxohept-3-en-3-olato-k2 O,O′)dysprosium(III), DyC43H67O6N2
Ling, Bo-Kai; Huang, Ling-Yu; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 831–833; doi:10.1515/ncrs-2023-0203

data_8107575
_publ_section_title
;
 Crystal structure of dipyridine-k1
 N-tris(2,2,6,6-tetramethyl-5-oxohept-3-en-3-olato-k2
 O,O&#x2032;)dysprosium(III), DyC43H67O6N2
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_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              831
_journal_page_last               833
_journal_paper_doi               10.1515/ncrs-2023-0203
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C43 H67 Dy N2 O6'
_chemical_formula_sum            'C43 H67 Dy N2 O6'
_chemical_formula_weight         870.48
_chemical_name_systematic        Dythd-py
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                94.903(4)
_cell_angle_beta                 98.580(4)
_cell_angle_gamma                105.417(4)
_cell_formula_units_Z            2
_cell_length_a                   10.384(3)
_cell_length_b                   13.502(4)
_cell_length_c                   16.972(5)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.45
_cell_volume                     2248.6(11)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25176
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.578
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0974 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.6694.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      .
_exptl_crystal_description       plate
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.413
_refine_diff_density_min         -2.457
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7762
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0130P)^2^+27.9048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7453
_reflns_number_total             7762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0203_suppl.cif
_cod_data_source_block           p1
_cod_database_code               8107575
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.629
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C32, C30, C33, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C30 \\sim C32 \\sim C31 \\sim C33: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C31A \\sim C32A \\sim C30A \\sim C33: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C22 \\sim C19 \\sim C21 \\sim C20: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) H32C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C30A(0.5) H30D(0.5)
 H30E(0.5) H30F(0.5) C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5) C32A(0.5)
 H32D(0.5) H32E(0.5) H32F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C6(H6), C17(H17), C38(H38), C28(H28), C39(H39), C34(H34), C42(H42),
 C40(H40), C35(H35), C37(H37), C41(H41), C36(H36)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C4(H4A,H4B,H4C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C1(H1A,H1B,H1C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C11(H11A,
 H11B,H11C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C),
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C30A(H30D,H30E,
 H30F), C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
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