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_7062613
_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 Ho2 N12 O2'
_chemical_formula_sum            'C48 H54 Ho2 N12 O2'
_chemical_formula_weight         1160.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 114.2700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4788(6)
_cell_length_b                   20.2131(8)
_cell_length_c                   16.9590(7)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      53.913
_cell_measurement_theta_min      2.952
_cell_volume                     4524.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II diffractrometer'
_computing_data_reduction        'SAINT V8.40B (?, 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      120.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54230
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.975
_diffrn_reflns_theta_min         4.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.926
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.3902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1593 before and 0.0958 after correction. The Ratio of minimum to maximum transmission is 0.5199. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'orangish red'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_recrystallization_method block
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.904
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0669P)^2^+4.4777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7928
_reflns_number_total             8166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02225k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062611--7062613.cif.'
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7062613
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.251
_shelx_estimated_absorpt_t_min   0.214
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Riding coordinates:
 N1(H1), N10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C16(H16a,H16b), C25(H25a,H25b), C35(H35a,H35b), C41(H41a,H41b),
 C42(H42a,H42b), C43(H43a,H43b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b),
  C47(H47a,H47b), C48(H48a,H48b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1a), C2(H2), C3(H3), C6(H6), C8(H8), C9(H9), C10(H10a), C11(H11),
 C12(H12), C13(H13), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C36(H36), C38(H38), C39(H39), C40(H40)
;
_olex2_submission_special_instructions 'No special instructions were received'