Unique and contrasting structures of homoleptic lanthanum(iii) and cerium(iii) 3,5-dimethylpyrazolates.
Werner, Daniel; Bayer, Uwe; Rad, Nazli E.; Junk, Peter C.; Deacon, Glen B.; Anwander, Reiner; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5952–5955; doi:10.1039/c8dt00338f

data_7045980
_publ_section_title
;
 Unique and contrasting structures of homoleptic lanthanum(iii) and
 cerium(iii) 3,5-dimethylpyrazolates.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5952
_journal_page_last               5955
_journal_paper_doi               10.1039/c8dt00338f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C60 H84 Ce4 N24'
_chemical_formula_sum            'C60 H84 Ce4 N24'
_chemical_formula_weight         1701.99
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5122(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3632(18)
_cell_length_b                   13.4207(11)
_cell_length_c                   25.122(2)
_cell_measurement_reflns_used    9381
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.099
_cell_measurement_theta_min      2.46
_cell_volume                     7081.8(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            106651
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         0.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.576
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1437 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.8665. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         19065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+5.7202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                15625
_reflns_number_total             19065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00338f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045977--7045980.cif.'
_cod_database_code               7045980
_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 Ternary CH refined with riding coordinates:
 C28(H28)
2.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C18(H18), C3(H3), C48(H48), C43(H43), C33(H33), C13(H13), C53(H53),
 C38(H38), C58(H58), C8(H8)
2.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C45(H45A,H45B,
 H45C), C16(H16A,H16B,H16C), C11(H11A,H11B,H11C), C46(H46A,H46B,H46C), C36(H36A,
 H36B,H36C), C15(H15A,H15B,H15C), C51(H51A,H51B,H51C), C5(H5A,H5B,H5C),
 C35(H35A,H35B,H35C), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C), C40(H40A,H40B,
 H40C), C56(H56A,H56B,H56C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C6(H6A,
 H6B,H6C), C60(H60A,H60B,H60C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'