Synthesis and comparison of iso-structural f-block metal complexes (Ce, U, Np, Pu) featuring <i>η</i><sup>6</sup>-arene interactions.
Murillo, Jesse; Goodwin, Conrad A. P.; Stevens, Lauren; Fortier, Skye; Gaunt, Andrew J.; Scott, Brian L.; Chemical science 14 (2023) 7438–7446; doi:10.1039/d3sc02194g

data_1569306
_publ_section_title
;
 Synthesis and comparison of iso-structural f-block metal complexes (Ce,
 U, Np, Pu) featuring <i>&#x3b7;</i><sup>6</sup>-arene interactions.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              7438
_journal_page_last               7446
_journal_paper_doi               10.1039/d3sc02194g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C100 H131.24 Ce2 Cl4 K2 N4 O5'
_chemical_formula_sum            'C100 H131.24 Ce2 Cl4 K2 N4 O5'
_chemical_formula_weight         1969.56
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-20
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3524(4)
_cell_length_b                   16.9877(5)
_cell_length_c                   25.6828(8)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.489
_cell_measurement_theta_min      2.526
_cell_volume                     5824.8(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            240020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         1.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0740 before and 0.0612 after correction. The Ratio of minimum to maximum transmission is 0.8270. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       plate
_exptl_crystal_F_000             2042
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         17795
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+11.5017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14935
_reflns_number_total             17795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           2_Ce
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_database_code               1569306
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Others
 Fixed Sof: C48(0.5) H2AA(0.5) H2AB(0.5) O3(0.5) O2(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) H1BD(0.5) H1BE(0.5) H1BF(0.5) O4(0.5) C53(0.5) H3AA(0.5) H3AB(0.5)
 C49(0.5) H4AA(0.5) H4AB(0.5) C52(0.5) H5AA(0.5) H5AB(0.5) C51(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) C47(0.5) H0AB(0.5) H0AC(0.5) H0AD(0.5)
 Fixed Uiso: H00A(0.032) H00C(0.034) H00I(0.044) H00J(0.034) H00L(0.038)
 H00N(0.033) H00Q(0.04) H00R(0.05) H00S(0.046) H00T(0.043) H00U(0.054)
 H00V(0.052) H00W(0.046) H00X(0.044) H00Y(0.044) H00Z(0.048) H010(0.053)
 H011(0.047) H012(0.053) H013(0.055) H014(0.047) H015(0.052) H01A(0.059)
 H01B(0.059) H01C(0.081) H01D(0.081) H01E(0.081) H01F(0.079) H01G(0.079)
 H01H(0.079) H01I(0.077) H01J(0.077) H01K(0.077) H01L(0.062) H01M(0.062)
 H01N(0.084) H01O(0.084) H01P(0.084) H01Q(0.082) H01R(0.082) H01S(0.082)
 H01T(0.097) H01U(0.097) H01V(0.097) H01W(0.107) H01X(0.107) H01Y(0.107)
 H01Z(0.136) H(0.136) HA(0.136) H01(0.083) HB(0.083) HC(0.083) H0AA(0.099)
 HD(0.099) HE(0.099) H3A(0.067) H3B(0.067) H3C(0.067) H4A(0.057) H4B(0.057)
 H4C(0.057) H2AA(0.082) H2AB(0.082) H1AA(0.103) H1AB(0.103) H1AC(0.103)
 H1BD(0.103) H1BE(0.103) H1BF(0.103) H3AA(0.125) H3AB(0.125) H4AA(0.094)
 H4AB(0.094) H5AA(0.127) H5AB(0.127) H9A(0.208) H9B(0.208) H9C(0.208)
 H0AB(0.175) H0AC(0.175) H0AD(0.175)
 Fixed X: H00A(0.396601) H00C(0.539028) H00I(0.383233) H00J(0.704228)
 H00L(0.29317) H00N(0.563348) H00Q(0.310004) H00R(1.025607) H00S(0.369722)
 H00T(0.159626) H00U(1.040788) H00V(0.926232) H00W(0.716325) H00X(0.925511)
 H00Y(0.171661) H00Z(0.553579) H010(0.721419) H012(0.585737) H013(0.86813)
 H014(0.465758) H015(0.970437) H01A(0.801702) H01B(0.887729) H01C(0.875044)
 H01D(0.777574) H01E(0.861318) H01F(0.387121) H01G(0.365021) H01H(0.471643)
 H01I(0.680013) H01J(0.666733) H01K(0.762839) H01L(0.762016) H01M(0.854326)
 H01N(0.221215) H01O(0.21294) H01P(0.235561) H01Q(0.806246) H01R(0.716103)
 H01S(0.824784) H01T(0.510852) H01U(0.557482) H01V(0.454636) H01W(0.716969)
 H01X(0.720599) H01Y(0.67619) H01Z(0.65618) H(0.750019) HA(0.745164)
 H01(0.95189) HB(0.960929) HC(1.036469) H0AA(0.991281) HD(0.894398)
 HE(0.885264) H3A(0.85967) H3B(0.814411) H3C(0.764403) H4A(1.030025)
 H4B(0.983886) H4C(1.030875) H2AA(0.766902) H2AB(0.818927) H1AA(0.879597)
 H1AB(0.966976) H1AC(0.931805) H1BD(0.86049) H1BE(0.976985) H1BF(0.894909)
 H3AA(0.946445) H3AB(0.929973) H4AA(0.901995) H4AB(0.93532) H5AA(0.836488)
 H5AB(0.836496) H9A(0.665877) H9B(0.692178) H9C(0.660927) H0AB(0.595812)
 H0AC(0.685082) H0AD(0.624201)
 Fixed Y: H00A(0.614268) H00C(0.684624) H00I(0.174047) H00J(0.569659)
 H00L(0.58022) H00N(0.499915) H00Q(0.312681) H00R(0.381769) H00S(0.384764)
 H00T(0.497264) H00U(0.372128) H00V(0.435234) H00W(0.776221) H00X(0.618254)
 H00Y(0.363311) H00Z(0.142363) H010(0.55701) H012(0.346875) H013(0.826411)
 H014(0.09042) H015(0.746554) H01A(0.103756) H01B(0.118893) H01C(0.562276)
 H01D(0.617102) H01E(0.626948) H01F(0.267228) H01G(0.358578) H01H(0.331463)
 H01I(0.432018) H01J(0.498561) H01K(0.442277) H01L(0.287763) H01M(0.249591)
 H01N(0.318668) H01O(0.347878) H01P(0.257287) H01Q(0.036148) H01R(0.023758)
 H01S(-0.010891) H01T(0.21542) H01U(0.292848) H01V(0.298145) H01W(0.256616)
 H01X(0.280226) H01Y(0.196658) H01Z(0.26056) H(0.310203) HA(0.217236)
 H01(0.571428) HB(0.517129) HC(0.504827) H0AA(0.368648) HD(0.380628)
 HE(0.334465) H3A(0.345013) H3B(0.40544) H3C(0.39764) H4A(0.509501)
 H4B(0.472199) H4C(0.416126) H2AA(0.073673) H2AB(-0.008362) H1AA(0.250505)
 H1AB(0.212324) H1AC(0.17036) H1BD(0.236761) H1BE(0.222681) H1BF(0.194914)
 H3AA(0.086529) H3AB(0.129106) H4AA(0.057288) H4AB(0.09867) H5AA(0.008986)
 H5AB(-0.02482) H9A(-0.016787) H9B(-0.062028) H9C(0.028891) H0AB(-0.033953)
 H0AC(-0.076438) H0AD(-0.006363)
 Fixed Z: H00A(0.641192) H00C(0.668607) H00I(0.705097) H00J(0.560857)
 H00L(0.537719) H00N(0.534004) H00Q(0.578413) H00R(0.676018) H00S(0.69477)
 H00T(0.514629) H00U(0.765892) H00V(0.818655) H00W(0.608031) H00X(0.711956)
 H00Y(0.534176) H00Z(0.579435) H010(0.774348) H012(0.550114) H013(0.641068)
 H014(0.648453) H015(0.692955) H01A(0.8669) H01B(0.825115) H01C(0.853671)
 H01D(0.85221) H01E(0.808812) H01F(0.774303) H01G(0.784107) H01H(0.762891)
 H01I(0.807895) H01J(0.851347) H01K(0.853124) H01L(0.804448) H01M(0.835914)
 H01N(0.66866) H01O(0.727674) H01P(0.715458) H01Q(0.765674) H01R(0.80516)
 H01S(0.818951) H01T(0.492291) H01U(0.466757) H01V(0.497705) H01W(0.57642)
 H01X(0.516158) H01Y(0.532942) H01Z(0.872646) H(0.894053) HA(0.903759)
 H01(0.603605) HB(0.552979) HC(0.601309) H0AA(0.58623) HD(0.549586)
 HE(0.603618) H3A(0.599084) H3B(0.557089) H3C(0.613062) H4A(0.605025)
 H4B(0.552687) H4C(0.596792) H2AA(0.586331) H2AB(0.602376) H1AA(0.703385)
 H1AB(0.669745) H1AC(0.722155) H1BD(0.675659) H1BE(0.68799) H1BF(0.728831)
 H3AA(0.685649) H3AB(0.630567) H4AA(0.677117) H4AB(0.623859) H5AA(0.608723)
 H5AB(0.667261) H9A(0.670139) H9B(0.617442) H9C(0.615661) H0AB(0.653481)
 H0AC(0.623581) H0AD(0.595998)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              50671
_shelx_fab_checksum              60425
_olex2_submission_special_instructions 'No special instructions were received'