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_7703023
_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, C28 H56 K O7, 4(C4 H8 O)'
_chemical_formula_sum            'C164 H244 Ce2 K2 O23'
_chemical_formula_weight         2942.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-09
_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                90
_cell_angle_beta                 92.6191(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6636(3)
_cell_length_b                   33.2740(6)
_cell_length_c                   27.8553(5)
_cell_measurement_reflns_used    25034
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.4620
_cell_measurement_theta_min      3.1180
_cell_volume                     16354.5(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000  -90.0000 50

  2 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000   90.0000 50

  3 omega  -93.00  -34.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767 -179.0000  120.0000 59

  4 omega  -43.00   55.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767   38.0000   60.0000 98

  5 omega  -90.00   56.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767    0.0000   30.0000 146

  6 omega  -90.00   56.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767    0.0000 -120.0000 146

  7 omega  -86.00  -61.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -57.0000 -150.0000 25

  8 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000 -150.0000 50

  9 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000    0.0000 50

 10 omega  -25.00   62.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  -99.0000  120.0000 87

 11 omega  -25.00   62.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  -99.0000  -60.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0019867000
_diffrn_orient_matrix_UB_12      0.0037097000
_diffrn_orient_matrix_UB_13      -0.0249879000
_diffrn_orient_matrix_UB_21      -0.0398351000
_diffrn_orient_matrix_UB_22      0.0027663000
_diffrn_orient_matrix_UB_23      -0.0018524000
_diffrn_orient_matrix_UB_31      0.0049330000
_diffrn_orient_matrix_UB_32      0.0208114000
_diffrn_orient_matrix_UB_33      0.0047010000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            113941
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         3.049
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             6264
_exptl_crystal_size_max          0.5196
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.0561
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         13888
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0859
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+276.0661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10626
_reflns_number_total             13888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           p15164peakhunting_monoclinic
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_database_code               7703023
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C156 H186 O12 Ce4'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H34A,H34B,H34C} of C340, All C(H,H) groups, All C(H,H,H,
  H) groups
 At 1.5 times of:
  {H12A,H12B,H12C} of C121, {H12D,H12E,H12F} of C122, {H22A,H22B,H22C} of
  C221, {H24A,H24B,H24C} of C240, {H32G,H32H,H32I} of C323, {H32D,H32E,H32F} of
  C322, {H12G,H12H,H12I} of C123, {H44A,H44B,H44C} of C440, {H22D,H22E,H22F} of
  C222, {H32A,H32B,H32C} of C321, {H22G,H22H,H22I} of C223, {H42D,H42E,H42F} of
  C422, {H42G,H42H,H42I} of C423, {H14A,H14B,H14C} of C140, {H42A,H42B,H42C} of
  C421
2. Restrained distances
 C69-C68
 1.44 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O7, C58, C59, C60, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, C76, C77, C78, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, C72, C73, C74, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C68, C69, C70, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C72, C73, C74, C75, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C79, O12, C76, C77, C78
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C60, C61, C58, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H55A(0.5) H55B(0.5) H55C(0.5) H55D(0.5) C56B(0.5) H56A(0.5)
 H56B(0.5) C56A(0.5) H56C(0.5) H56D(0.5) H57C(0.5) H57D(0.5) H57B(0.5) H57A(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C55(H55C,H55D), C56B(H56A,H56B), C56A(H56C,H56D),
 C57(H57C,H57D), C57(H57B,H57A), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
  C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,
 H65B), C66(H66A,H66B), C67(H67A,H67B), C72(H72A,H72B), C73(H73A,H73B),
 C74(H74A,H74B), C75(H75A,H75B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C76(H76A,H76B), C77(H77B,H77A), C78(H78A,H78B), C79(H79A,H79B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C13(H13), C15(H15), C23(H23), C25(H25),
 C33(H33), C35(H35), C43(H43), C45(H45)
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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'