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_7043772
_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         'C114 H152 La6 N28 O13'
_chemical_formula_sum            'C119 H159 La6 N30 O13'
_chemical_formula_weight         3051.16
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   61.727(6)
_cell_length_b                   61.727(6)
_cell_length_c                   12.5925(18)
_cell_measurement_reflns_used    8375
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      15.27
_cell_measurement_theta_min      2.29
_cell_volume                     41552(8)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0693
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            28804
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        15.290
_diffrn_reflns_theta_max         15.290
_diffrn_reflns_theta_min         0.660
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction wR2(int)'
 was0.1163 before and 0.0521 after correction. The Ratio of minimum to maximum 
transmission is 0.8201. 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    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13662
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details          TITL
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     755
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+1058.6670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3253
_reflns_number_total             3956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00635g2.cif
_cod_data_source_block           6c
_cod_original_cell_volume        41552(10)
_cod_database_code               7043772
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C42-C41
 1.51 with sigma of 0.02
 C40-C42
 2.67 with sigma of 0.02
 C56-C55
 1.51 with sigma of 0.01
 C55-C54
 1.51 with sigma of 0.01
 C54-C53
 1.51 with sigma of 0.01
 N14-C47
 2.47 with sigma of 0.02
 C47-C46
 1.47 with sigma of 0.02
 C47-C45
 2.6 with sigma of 0.02
 C43-C45
 2.6 with sigma of 0.02
 C43-N13
 2.47 with sigma of 0.02
 C43-C44
 1.47 with sigma of 0.02
 C44-C45
 1.4 with sigma of 0.02
 C44-N13
 1.3 with sigma of 0.02
 C58-C59
 1.51 with sigma of 0.01
3. Restrained planarity
 C38, C39, N12, N11, C41, C40
 with sigma of 0.1
 C42, C41, N11, N12, C39, C40, C38
 with sigma of 0.1
 C47, C43, C46, C45, C44, N13, N14
 with sigma of 0.1
 C43, C44, C45, N13, C46, N14, C47
 with sigma of 0.1
4. 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
5. Others
 Fixed Sof: H37(0.5) N12(0.5) C40(0.5) H40(0.5) C39(0.5) O5(0.5) N11(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C53(0.5) H53(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C41(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5) C55(0.5) H55A(0.5) H55B(0.5) C45(0.5) H45(0.5) C46(0.5) N14(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) N13(0.5) C44(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) H43C(0.5)
6.a Riding coordinates:
 C5(H5A,H5B,H5C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C27(H27A,H27B,
 H27C), C48(H48A,H48B,H48C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C16(H16A,
 H16B,H16C), C12(H12A,H12B,H12C), C52(H52A,H52B,H52C), C22(H22A,H22B,H22C),
 C1(H1A,H1B,H1C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C),
  C43(H43A,H43B,H43C)
6.b Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C64(H64A,H64B), C63(H63A,H63B), C62(H62A,H62B), C60(H60A,
 H60B), C59(H59A,H59B), C57(H57A,H57B), C58(H58A,H58B), C56(H56A,H56B),
 C54(H54A,H54B), C55(H55A,H55B)
6.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C29(H29), C24(H24), C10(H10), C7(H7), C9(H9), C37(H37), C3(H3),
 C8(H8), C34(H34), C33(H33), C50(H50), C19(H19), C14(H14), C40(H40), C53(H53),
 C45(H45)
;
_shelx_res_checksum              63434
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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