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_7043776
_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         'C138 H174 La8 N40 O12, 4(C7 H8)'
_chemical_formula_sum            'C166 H206 La8 N40 O12'
_chemical_formula_weight         4064.98
_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     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                 96.918(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.978(3)
_cell_length_b                   36.827(6)
_cell_length_c                   14.593(3)
_cell_measurement_reflns_used    1381
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      18.29
_cell_measurement_theta_min      2.44
_cell_volume                     8524(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  0.2438
_diffrn_reflns_av_unetI/netI     0.2311
_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       39
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43140
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.497
_diffrn_reflns_theta_min         1.398
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.2308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1625 before and 0.0970 after correction. The Ratio of minimum to maximum transmission is 0.3098. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       plate
_exptl_crystal_F_000             4068
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1669
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5805
_reflns_number_total             11143
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {55c95537-95f3-4aa7-a2ed-5d4f1180b7e2}
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           6a
_cod_original_cell_volume        8525(3)
_cod_database_code               7043776
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C71) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C29) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C45) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C73) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C57) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C56) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C108(H10A,H10B), C2AA(H2AA,H2AB), C91(H91A,H91B), C166(H16D,H16E)
3.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C3(H3), C66(H66), C76(H76), C9(H9), C8(H8), C45(H45), C19(H19),
 C37(H37), C75(H75), C33(H33), C24(H24), C71(H71), C10(H10), C79(H79), C29(H29),
  C14(H14), C48(H48), C7(H7), C67(H67), C43(H43), C69(H69), C68(H68), C53(H53),
 C58(H58), C40(H40), C63(H63), C78(H78), C77(H77)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C1(H1A,H1B,H1C), C42(H42A,H42B,H42C), C5(H5A,H5B,H5C),
 C60(H60A,H60B,H60C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C), C31(H31A,H31B,H31C), C65(H65A,H65B,H65C), C50(H50A,H50B,H50C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C38(H38A,H38B,H38C),
 C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C61(H61A,H61B,H61C), C56(H56A,H56B,
 H56C), C73(H73A,H73B,H73C), C46(H46A,H46B,H46C), C72(H72A,H72B,H72C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;