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_7045977
_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, C7 H8'
_chemical_formula_sum            'C67 H92 Ce4 N24'
_chemical_formula_weight         1794.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-25 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                103.244(4)
_cell_angle_beta                 91.321(7)
_cell_angle_gamma                90.869(5)
_cell_formula_units_Z            2
_cell_length_a                   14.583(4)
_cell_length_b                   15.851(4)
_cell_length_c                   16.822(4)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.42
_cell_volume                     3783.2(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1314
_diffrn_reflns_av_unetI/netI     0.1144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62514
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         1.244
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1425 before and 0.0767 after correction. The Ratio of minimum to maximum transmission is 0.6576. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.866
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.206
_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     879
_refine_ls_number_reflns         12597
_refine_ls_number_restraints     1344
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0357P)^2^+10.1624P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8655
_reflns_number_total             12597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00338f2.cif
_cod_data_source_block           2PhMe
_cod_depositor_comments
'Adding full bibliography for 7045977--7045980.cif.'
_cod_original_cell_volume        3783.0(17)
_cod_database_code               7045977
_shelxl_version_number           2013-2
_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. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C28(H28)
4.b Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C31(H31A,H31B,H31C)
4.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C33(H33), C13(H13), C8(H8), C18(H18), C53(H53), C48(H48), C43(H43),
 C38(H38), C58(H58), C7S(H7S), C6S(H6S), C5S(H5S), C3(H3), C3S(H3S), C4S(H4S)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C55(H55A,H55B,H55C), C30(H30A,H30B,H30C), C6(H6A,H6B,H6C), C51(H51A,
 H51B,H51C), C45(H45A,H45B,H45C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C1S(H1SA,H1SB,H1SC), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C26(H26A,H26B,
 H26C), C11(H11A,H11B,H11C), C60(H60A,H60B,H60C), C50(H50A,H50B,H50C), C20(H20A,
 H20B,H20C), C46(H46A,H46B,H46C), C5(H5A,H5B,H5C), C36(H36A,H36B,H36C), C1(H1A,
 H1B,H1C)
;
_shelx_res_checksum              82361
_olex2_submission_special_instructions 'No special instructions were received'