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_7043774
_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         'C65 H87 Ce3 N18 O6, 3.5(C4 H8 O)'
_chemical_formula_sum            'C79 H115 Ce3 N18 O9.5'
_chemical_formula_weight         1889.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6971(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9544(4)
_cell_length_b                   18.6568(4)
_cell_length_c                   26.6336(6)
_cell_measurement_reflns_used    8156
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.456
_cell_measurement_theta_min      2.434
_cell_volume                     8499.3(3)
_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      100.15
_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  0.0996
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.999
_diffrn_reflns_theta_max         19.999
_diffrn_reflns_theta_min         1.355
_exptl_absorpt_coefficient_mu    1.644
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.5702.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             3860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         7931
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0540P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5140
_reflns_number_total             7931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           5a3thf
_cod_original_formula_sum        'C79 H115 Ce3 N18 O9.50'
_cod_database_code               7043774
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2Aa,H2Ab} of C2AA, {H1Ba,H1Bb} of C1BA, {H85a,H85b} of
  C85, {H87a,H87b} of C87, {H14a,H14b} of C142, {H14c,H14d} of C144, {H17d,
  H17e} of C175, {H18a,H18b} of C183, {H2Sa,H2Sb} of C2S, {H3Sa,H3Sb} of C3S,
  {H4Sa,H4Sb} of C4S, {H5Sa,H5Sb} of C5S, {H7Sa,H7Sb} of C7S, {H8Sa,H8Sb} of
  C8S, {H9Sa,H9Sb} of C9S, {H10a,H10b} of C10S, {H12d,H12e} of C12S, {H13a,
  H13b} of C13S, {H14e,H14f} of C14S, {H15a,H15b} of C15S
 At 1.5 times of:
  All C(H,H,H) groups, {H17f,H17g} of C17S, {H18c,H18d} of C18S
 At 1.3 times of:
  {H19a,H19b} of C19S
2. 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
3. Others
 Fixed Sof: O16S(0.5) C17S(0.5) H17f(0.5) H17g(0.5) C19S(0.5) H19a(0.5)
 H19b(0.5)
4.a Riding coordinates:
 C17S(H17f,H17g), C19S(H19a,H19b), C18S(H18c,H18d)
4.b Secondary CH2 refined with riding coordinates:
 C1BA(H1Ba,H1Bb), C2AA(H2Aa,H2Ab), C85(H85a,H85b), C87(H87a,H87b), C142(H14a,
 H14b), C144(H14c,H14d), C175(H17d,H17e), C183(H18a,H18b), C2S(H2Sa,H2Sb),
 C3S(H3Sa,H3Sb), C4S(H4Sa,H4Sb), C5S(H5Sa,H5Sb), C7S(H7Sa,H7Sb), C8S(H8Sa,H8Sb),
  C9S(H9Sa,H9Sb), C10S(H10a,H10b), C12S(H12d,H12e), C13S(H13a,H13b), C14S(H14e,
 H14f), C15S(H15a,H15b)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C19(H19), C23(H23),
 C24(H24), C25(H25), C26(H26), C30(H30), C35(H35), C40(H40), C45(H45), C50(H50),
  C55(H55)
4.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C12(H12a,H12b,H12c), C16(H16a,H16b,H16c),
 C17(H17a,H17b,H17c), C21(H21a,H21b,H21c), C28(H28a,H28b,H28c), C32(H32a,H32b,
 H32c), C33(H33a,H33b,H33c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C42(H42a,
 H42b,H42c), C43(H43a,H43b,H43c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c),
 C52(H52a,H52b,H52c), C53(H53a,H53b,H53c), C57(H57a,H57b,H57c)
;
_shelx_res_checksum              80453
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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