Organolanthanide η1- and η5-pyrrolyl half-sandwich compounds: synthesis, structures, and magnetic properties
She, Yeye; Lu, Yanhua; Jia, Chaohong; Li, Yahong; Zhang, Yi-Quan; Yao, Jin-lei; New Journal of Chemistry 47 (2023) 15650–15657; doi:10.1039/D3NJ02225K

data_7062612
_publ_section_title
;
 Organolanthanide \h1- and \h5-pyrrolyl half-sandwich compounds:
 synthesis, structures, and magnetic properties
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15650
_journal_page_last               15657
_journal_paper_doi               10.1039/D3NJ02225K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C48 H54 Dy2 N12 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H70 Dy2 N12 O4'
_chemical_formula_weight         1300.24
_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
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                95.8290(10)
_cell_angle_beta                 102.2810(10)
_cell_angle_gamma                95.0500(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5631(4)
_cell_length_b                   12.6486(4)
_cell_length_c                   19.3347(6)
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.02
_cell_volume                     2731.30(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX II diffractrometer'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.02
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52314
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         2.173
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.772
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1239 before and 0.0709 after correction. The Ratio of minimum to maximum transmission is 0.7995. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         12414
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+5.8185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11269
_reflns_number_total             12414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02225k2.cif
_cod_data_source_block           q
_cod_depositor_comments
'Adding full bibliography for 7062611--7062613.cif.'
_cod_database_code               7062612
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.621
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C42A) \\sim Ueq, Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C43A) \\sim Ueq, Uanis(C43B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C47A) = Uanis(C47B)
Uanis(C43A) = Uanis(C43B)
Uanis(C42A) = Uanis(C42B)
3. Others
 Sof(H41C)=Sof(H41D)=Sof(H48C)=Sof(H48D)=Sof(H44C)=Sof(H44D)=Sof(C42B)=
 Sof(H42A)=Sof(H42B)=Sof(H46C)=Sof(H46D)=Sof(C47B)=Sof(H47A)=Sof(H47B)=
 Sof(C43B)=Sof(H43A)=Sof(H43B)=1-FVAR(1)
 Sof(H41A)=Sof(H41B)=Sof(H48A)=Sof(H48B)=Sof(H44A)=Sof(H44B)=Sof(H46A)=
 Sof(H46B)=Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=
 Sof(C42A)=Sof(H42C)=Sof(H42D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C29(H29), C30(H30), C28(H28)
4.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C36(H36A,H36B), C15(H15A,H15B), C53(H53A,H53B), C49(H49A,
 H49B), C55(H55A,H55B), C6(H6A,H6B), C54(H54A,H54B), C26(H26A,H26B), C41(H41C,
 H41D), C41(H41A,H41B), C50(H50A,H50B), C52(H52A,H52B), C45(H45A,H45B),
 C48(H48C,H48D), C48(H48A,H48B), C44(H44C,H44D), C44(H44A,H44B), C42B(H42A,
 H42B), C51(H51A,H51B), C46(H46C,H46D), C46(H46A,H46B), C47B(H47A,H47B),
 C43B(H43A,H43B), C47A(H47C,H47D), C43A(H43C,H43D), C42A(H42C,H42D)
4.c Aromatic/amide H refined with riding coordinates:
 C35(H35), N12(H12A), C22(H22), C38(H38), C19(H19), N3(H3), C1(H1), C3(H3A),
 C39(H39), C2(H2), C21(H21), C25(H25), C31(H31), C33(H33), C5(H5), C32(H32),
 C16(H16), C8(H8), C18(H18), C40(H40), C10(H10), C23(H23), C9(H9), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'