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_7703021
_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         'C52 H63 Ce Cl N4 O2, C4 H8 O, 3(C5 H5 N)'
_chemical_formula_sum            'C71 H86 Ce Cl N7 O3'
_chemical_formula_weight         1261.03
_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     dual
_audit_creation_date             2019-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-12 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                76.0300(10)
_cell_angle_beta                 80.3200(10)
_cell_angle_gamma                61.8470(10)
_cell_formula_units_Z            2
_cell_length_a                   13.9455(2)
_cell_length_b                   14.0906(2)
_cell_length_c                   20.0971(3)
_cell_measurement_reflns_used    27135
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.5720
_cell_measurement_theta_min      3.2070
_cell_volume                     3372.09(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -87.00   6.00   1.00   30.00    --  -16.31 -38.00 120.00   93
  2  \w    -25.00  24.00   1.00   30.00    --  -16.31 -99.00 -90.00   49
  3  \w    -35.00  52.00   1.00   30.00    --  -16.31  57.00 -90.00   87
  4  \w    -35.00  52.00   1.00   30.00    --  -16.31  57.00 150.00   87
  5  \w    -25.00  24.00   1.00   30.00    --  -16.31 -99.00-120.00   49
  6  \w    -25.00  24.00   1.00   30.00    --  -16.31 -99.00  30.00   49
  7  \w      0.00  86.00   1.00   30.00    --   18.03  57.00  60.00   86
  8  \w    -20.00  90.00   1.00   30.00    --   18.03  19.00  30.00  110
  9  \w    -85.00   2.00   1.00   30.00    --  -16.31 -57.00-120.00   87
 10  \w    -25.00  59.00   1.00   30.00    --   18.03 -99.00 -60.00   84
 11  \w    -25.00  59.00   1.00   30.00    --   18.03 -99.00-180.00   84
 12  \w      0.00  49.00   1.00   30.00    --   18.03  57.00 150.00   49
 13  \w    -50.00  37.00   1.00   30.00    --   18.03 -57.00  30.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74594
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.377
_diffrn_reflns_theta_min         2.910
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         16549
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+1.8351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13910
_reflns_number_total             16549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           p16191
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_database_code               7703021
_shelx_shelxl_version_number     2018/3
_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. Rigid body (RIGU) restrains
 C51, C50, C49, C48, C47, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6AA, C900, C901, C902, C903
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C3AA)=Sof(H3AA)=Sof(N913)=Sof(C914)=Sof(H914)=Sof(C915)=Sof(H915)=
 Sof(C916)=Sof(H916)=Sof(C2AA)=Sof(H2AA)=1-FVAR(1)
 Sof(C909)=Sof(H909)=Sof(C904)=Sof(H904)=Sof(C905)=Sof(H905)=Sof(N906)=
 Sof(C907)=Sof(H907)=Sof(C908)=Sof(H908)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C901(H90A,H90B), C900(H90C,H90D), C903(H90E,H90F), C902(H90G,H90H)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C10(H10), C22(H22), C23(H23), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C909(H909), C904(H904),
 C905(H905), C907(H907), C908(H908), C3AA(H3AA), C914(H914), C915(H915),
 C916(H916), C2AA(H2AA)
4.d Fitted hexagon refined as free rotating group:
 C909(C904,C905,N906,C907,C908), C3AA(N913,C914,C915,C916,C2AA)
4.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;