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_7058990
_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         '2(C63 H50 Dy K O9)'
_chemical_formula_sum            'C126 H100 Dy2 K2 O18'
_chemical_formula_weight         2305.25
_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     direct
_audit_creation_date             2018-11-27
_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                 104.6080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.8124(5)
_cell_length_b                   28.9292(5)
_cell_length_c                   26.2157(5)
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.23
_cell_volume                     21144.9(7)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            136904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.762
_diffrn_reflns_theta_min         1.014
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0753 before and 0.0529 after correction. The Ratio of minimum to maximum transmission is 0.7206. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       prism
_exptl_crystal_F_000             9360
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1341
_refine_ls_number_reflns         27414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+46.7923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23488
_reflns_number_total             27414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02059d2.cif
_cod_data_source_block           ts209_3b_2
_cod_database_code               7058990
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C32(H32), C42(H42), C112(H112), C113(H113), C114(H114),
 C115(H115), C116(H116), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C212(H212), C213(H213), C214(H214), C215(H215), C216(H216),
 C222(H222), C223(H223), C224(H224), C225(H225), C226(H226), C312(H312),
 C313(H313), C314(H314), C315(H315), C316(H316), C322(H322), C323(H323),
 C324(H324), C325(H325), C326(H326), C412(H412), C413(H413), C414(H414),
 C415(H415), C416(H416), C422(H422), C423(H423), C424(H424), C425(H425),
 C426(H426), C52(H52), C62(H62), C72(H72), C82(H82), C512(H512), C513(H513),
 C514(H514), C515(H515), C516(H516), C522(H522), C523(H523), C524(H524),
 C525(H525), C526(H526), C612(H612), C613(H613), C614(H614), C615(H615),
 C616(H616), C622(H622), C623(H623), C624(H624), C625(H625), C626(H626),
 C712(H712), C713(H713), C714(H714), C715(H715), C716(H716), C722(H722),
 C723(H723), C724(H724), C725(H725), C726(H726), C812(H812), C813(H813),
 C814(H814), C815(H815), C816(H816), C822(H822), C823(H823), C824(H824),
 C825(H825), C826(H826)
2.b Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C97(H97A,H97B,
 H97C)
;
_shelx_res_checksum              56612
_olex2_submission_special_instructions 'No special instructions were received'