A fresh look at the structural diversity of dibenzoylmethanide complexes of lanthanides
Sukhikh, Taisiya S.; Kolybalov, Dmitry S.; Pylova, Ekaterina K.; Bashirov, Denis A.; Komarov, Vladislav Y.; Kuratieva, Natalia V.; Smolentsev, Anton I.; Fitch, Andrew N.; Konchenko, Sergey N.; New Journal of Chemistry 43 (2019) 9934–; doi:10.1039/C9NJ02059D

data_7058986
_publ_section_title
;
 A fresh look at the structural diversity of dibenzoylmethanide complexes
 of lanthanides
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9934
_journal_paper_doi               10.1039/C9NJ02059D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C45 H33 Dy1 O7'
_chemical_formula_sum            'C45 H35 Dy O7'
_chemical_formula_weight         850.23
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-18 deposited with the CCDC.	2019-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.7056(10)
_cell_length_b                   22.7056(10)
_cell_length_c                   6.3514(3)
_cell_measurement_reflns_used    5629
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      3.11
_cell_volume                     2835.7(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5976
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.809
_diffrn_reflns_theta_max         25.809
_diffrn_reflns_theta_min         3.108
_exptl_absorpt_coefficient_mu    2.028
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1129 before and 0.0578 after correction. The Ratio of minimum to maximum transmission is 0.8371. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       prism
_exptl_crystal_F_000             1281
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 893 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2087
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.1024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.737
_reflns_Friedel_fraction_max     0.736
_reflns_number_gt                2087
_reflns_number_total             2087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02059d2.cif
_cod_data_source_block           kds36_1
_cod_original_cell_volume        2835.7(3)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7058986
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.462
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              57110
_olex2_submission_special_instructions 'No special instructions were received'