Dicerium letterbox-shaped tetraphenolates: f-block complexes designed for two-electron chemistry.
Arnold, Polly L.; Wang, Kai; Gray, Steven J.; Moreau, Liane M.; Booth, Corwin H.; Curcio, Massimiliano; Wells, Jordann A. L.; Slawin, Alexandra M. Z.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 877–884; doi:10.1039/c9dt03291f

data_7703020
_publ_section_title
;
 Dicerium letterbox-shaped tetraphenolates: f-block complexes designed for
 two-electron chemistry.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              877
_journal_page_last               884
_journal_paper_doi               10.1039/c9dt03291f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C120 H156 Ce2 K O12, 0.5(C12 H24 K O6), C10 H20 K0.5 O4'
_chemical_formula_sum            'C136 H188 Ce2 K2 O19'
_chemical_formula_weight         2485.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                112.342(3)
_cell_angle_beta                 91.967(3)
_cell_angle_gamma                92.513(2)
_cell_formula_units_Z            2
_cell_length_a                   21.7935(6)
_cell_length_b                   23.1848(7)
_cell_length_c                   24.6660(10)
_cell_measurement_reflns_used    21271
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.5470
_cell_measurement_theta_min      3.1630
_cell_volume                     11499.0(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
  1 omega  -44.00  -18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089   77.0000 -120.0000 26

  2 omega  -66.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089 -179.0000   30.0000 32

  3 omega  -25.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -99.0000  120.0000 49

  4 omega  -83.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -57.0000  -30.0000 83

  5 omega  -85.00  -58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3089  -57.0000  -60.0000 27

  6 omega   52.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  179.0000 -180.0000 40

  7 omega  -10.00   21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277   77.0000  -30.0000 31

  8 omega  -50.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  -57.0000   90.0000 58

  9 omega  -47.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0277  -38.0000 -180.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0244290000
_diffrn_orient_matrix_UB_12      0.0208435000
_diffrn_orient_matrix_UB_13      -0.0008302000
_diffrn_orient_matrix_UB_21      0.0036092000
_diffrn_orient_matrix_UB_22      -0.0188448000
_diffrn_orient_matrix_UB_23      -0.0299030000
_diffrn_orient_matrix_UB_31      -0.0213249000
_diffrn_orient_matrix_UB_32      0.0175677000
_diffrn_orient_matrix_UB_33      -0.0086408000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.1527
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            96714
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.462
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.718
_exptl_crystal_description       block
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.7227
_exptl_crystal_size_mid          0.5537
_exptl_crystal_size_min          0.4425
_refine_diff_density_max         2.982
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1548
_refine_ls_number_reflns         50114
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1061
_refine_ls_shift/su_max          0.426
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1410P)^2^+32.5892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2670
_refine_ls_wR_factor_ref         0.3166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26998
_reflns_number_total             50114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           p16002
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_original_cell_volume        11498.9(7)
_cod_database_code               7703020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C70 H70 O8 Ce2 K1'
_reflns_odcompleteness_completeness 95.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 C953-O19
 1.45 with sigma of 0.02
 O22-C958 = O18-C951 = O18-C952 = O15_$2-C920_$2 = O15_$2-C921_$2 = O16_$2-
 C922_$2 = O16_$2-C923_$2 = O17_$2-C924_$2
 1.45 with sigma of 0.02
 C959-O22
 1.45 with sigma of 0.02
 C951-C950 = C953-C952 = C958-C957 = C960-C959 = C924_$2-C923_$2 = C922_$2-
 C921_$2
 1.5 with sigma of 0.02
 C955-C954
 1.45 with sigma of 0.02
 O19-C954
 1.46 with sigma of 0.02
 C959-C958
 2.5 with sigma of 0.02
 C955_$1-C950
 2.5 with sigma of 0.02
 C955-C950_$1
 2.5 with sigma of 0.02
 O18-C950
 2.5 with sigma of 0.02
 O21-C955
 2.5 with sigma of 0.02
 C956-C955
 1.48 with sigma of 0.02
 O20-C955
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C2A, C3A, C4A, C5A, C6A, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C50, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C958, O22, C959
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O20(0.5) O21(0.5) O22(0.5) C957(0.5) H95A(0.5) H95B(0.5) C958(0.5)
 H95C(0.5) H95D(0.5) C959(0.5) H95E(0.5) H95F(0.5) C960(0.5) H96A(0.5)
 H96B(0.5) O18(0.5) O19(0.5) C950(0.5) H95G(0.5) H95H(0.5) C951(0.5) H95I(0.5)
 H95J(0.5) C952(0.5) H95K(0.5) H95L(0.5) C953(0.5) H95M(0.5) H95N(0.5)
 C955(0.5) H95O(0.5) H95P(0.5) C954(0.5) H95Q(0.5) H95R(0.5) O70(0.5) C956(0.5)
 H95S(0.5) H95T(0.5) C961(0.5) H96C(0.5) H96D(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C8(H8), C8A(H8A)
5.b Secondary CH2 refined with riding coordinates:
 C900(H90A,H90B), C901(H90C,H90D), C902(H90E,H90F), C903(H90G,H90H), C904(H90I,
 H90J), C905(H90K,H90L), C906(H90M,H90N), C907(H90O,H90P), C908(H90Q,H90R),
 C909(H90S,H90T), C910(H91A,H91B), C911(H91C,H91D), C912(H91E,H91F), C913(H91G,
 H91H), C914(H91I,H91J), C915(H91K,H91L), C957(H95A,H95B), C958(H95C,H95D),
 C959(H95E,H95F), C960(H96A,H96B), C950(H95G,H95H), C951(H95I,H95J), C952(H95K,
 H95L), C953(H95M,H95N), C916(H91M,H91N), C917(H91O,H91P), C918(H91Q,H91R),
 C919(H91S,H91T), C920(H92A,H92B), C921(H92C,H92D), C922(H92E,H92F), C923(H92G,
 H92H), C924(H92I,H92J), C925(H92K,H92L), C955(H95O,H95P), C954(H95Q,H95R),
 C956(H95S,H95T), C961(H96C,H96D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C4(H4), C4A(H4A), C6(H6), C6A(H6A), C7(H7), C7A(H7A),
 C13(H13), C15(H15), C23(H23), C25(H25), C33(H33), C35(H35), C43(H43), C45(H45),
  C53(H53), C55(H55), C63(H63), C65(H65), C73(H73), C75(H75), C82(H82), C84(H84)
5.d Idealised Me refined as rotating group:
 C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C140(H14A,
 H14B,H14C), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F), C223(H22G,H22H,H22I),
 C240(H24A,H24B,H24C), C321(H32A,H32B,H32C), C322(H32D,H32E,H32F), C323(H32G,
 H32H,H32I), C340(H34A,H34B,H34C), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F),
 C423(H42G,H42H,H42I), C440(H44A,H44B,H44C), C521(H52A,H52B,H52C), C522(H52D,
 H52E,H52F), C523(H52G,H52H,H52I), C540(H54A,H54B,H54C), C621(H62A,H62B,H62C),
 C622(H62D,H62E,H62F), C623(H62G,H62H,H62I), C640(H64A,H64B,H64C), C721(H72A,
 H72B,H72C), C722(H72D,H72E,H72F), C723(H72G,H72H,H72I), C740(H74A,H74B,H74C),
 C821(H82A,H82B,H82C), C822(H82D,H82E,H82F), C823(H82G,H82H,H82I), C840(H84A,
 H84B,H84C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'