Pyrazolates advance cerium chemistry: a Ce(III)/Ce(IV) redox equilibrium with benzoquinone.
Werner, Daniel; Deacon, Glen B.; Junk, Peter C.; Anwander, Reiner; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00635g

data_7043775
_publ_section_title
;
 Pyrazolates advance cerium chemistry: a Ce(III)/Ce(IV) redox equilibrium
 with benzoquinone.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00635g
_journal_year                    2017
_chemical_formula_moiety         'C44 H76 Ce N8'
_chemical_formula_sum            'C44 H76 Ce N8'
_chemical_formula_weight         857.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0706(17)
_cell_length_b                   12.7480(11)
_cell_length_c                   18.5268(16)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    173.10
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.66
_cell_volume                     4740.3(7)
_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      173.10
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0857
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60849
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         3.666
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1223 before and 0.0666 after correction. The Ratio of minimum to maximum transmission is 0.8038. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 4849 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.008(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         11741
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0391
_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^)+6.5260P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11290
_reflns_number_total             11741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           4
_cod_database_code               7043775
_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. Restrained distances
 C4-C10A \\sim C10B-C1 \\sim C7AA-C10B \\sim C6AA-C10A \\sim C17C-C10A \\sim
C17C-C10B
 with sigma of 0.02
 C14-C10B \\sim C14-C10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uiso(C10A) = Uiso(C10B)
4. Others
 Fixed Sof: C10B(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C7AA(0.5)
 H7AA(0.5) H7AB(0.5) H7AC(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) H4C(0.5) C10A(0.5)
5.a Riding coordinates:
 C17C(H17A,H17B,H17C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C18(H18), C13(H13), C8(H8)
5.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C0AA(H0AA,H0AB,H0AC), C41(H41A,H41B,H41C), C39(H39A,H39B,
 H39C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C2AA(H2AA,H2AB,H2AC),
 C32(H32A,H32B,H32C), C69(H69A,H69B,H69C), C35(H35A,H35B,H35C), C33(H33A,H33B,
 H33C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C21(H21A,
 H21B,H21C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C),
 C40(H40A,H40B,H40C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C6AA(H6AA,H6AB,
 H6AC), C7AA(H7AA,H7AB,H7AC), C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              1644
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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