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_7058989
_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         'C150 H112 Nd4 O22, C7 H8'
_chemical_formula_sum            'C157 H120 Nd4 O22'
_chemical_formula_weight         2935.47
_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             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                78.7490(10)
_cell_angle_beta                 66.6210(10)
_cell_angle_gamma                74.1200(10)
_cell_formula_units_Z            1
_cell_length_a                   15.0415(5)
_cell_length_b                   15.0538(6)
_cell_length_c                   16.1542(6)
_cell_measurement_reflns_used    8781
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.39
_cell_volume                     3213.8(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25267
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.195
_diffrn_reflns_theta_min         1.511
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0370 before and 0.0323 after correction.
The Ratio of minimum to maximum transmission is 0.9290.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         14199
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0538P)^2^+11.9606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10424
_reflns_number_total             14199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02059d2.cif
_cod_data_source_block           por006a
_cod_database_code               7058989
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.732
_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. Restrained distances
 C531-C53 \\sim C521-C53
 with sigma of 0.02
3. Rigid bond restraints
 C531, C532, C533, C534, C535, C536
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C521, C522, C523, C524, C525, C526
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C111, C112, C113, C114, C115, C116
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C521 \\sim C522 \\sim C523 \\sim C524 \\sim C525 \\sim C526: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C531 \\sim C532 \\sim C533 \\sim C534 \\sim C535 \\sim C536: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C1S) = Uiso(C2S) = Uiso(C3S) = Uiso(C4S) = Uiso(C5S) = Uiso(C6S)
5. Others
 Sof(C531)=Sof(C536)=Sof(H536)=Sof(C535)=Sof(H535)=Sof(C534)=Sof(H534)=
 Sof(C533)=Sof(H533)=Sof(C532)=Sof(H532)=1-FVAR(1)
 Sof(C521)=Sof(C522)=Sof(H522)=Sof(C523)=Sof(H523)=Sof(C524)=Sof(H524)=
 Sof(C525)=Sof(H525)=Sof(C526)=Sof(H526)=FVAR(1)
 Fixed Sof: C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5) C1S(0.5) C2S(0.5) H2S(0.5)
 C3S(0.5) H3S(0.5) C4S(0.5) H4S(0.5) C5S(0.5) H5S(0.5) C6S(0.5) H6S(0.5)
6.a Free rotating group:
 C7S(C1S,C2S,C3S,C4S,C5S,C6S)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C32(H32), C42(H42), C52(H52), C1AA(H1AA), C2AA(H2AA),
 C3AA(H3AA), C4AA(H4AA), C5AA(H5AA), 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), C512(H512), C513(H513), C514(H514),
 C515(H515), C516(H516), C522(H522), C523(H523), C524(H524), C525(H525),
 C526(H526), C536(H536), C535(H535), C534(H534), C533(H533), C532(H532),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116)
6.c Fitted hexagon refined as free rotating group:
 C521(C522,C523,C524,C525,C526), C531(C536,C535,C534,C533,C532)
6.d Idealised Me refined with riding coordinates:
 C7S(H7SA,H7SB,H7SC)
;
_shelx_res_checksum              51897
_olex2_submission_special_instructions 'No special instructions were received'