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_7703025
_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         'C64 H86 O4'
_chemical_formula_sum            'C64 H86 O4'
_chemical_formula_weight         919.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-08
_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                 97.547(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9580(6)
_cell_length_b                   18.2710(10)
_cell_length_c                   14.4742(7)
_cell_measurement_reflns_used    5590
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      21.1930
_cell_measurement_theta_min      3.0470
_cell_volume                     2872.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  22.00   1.00   15.00    --  -18.53 -99.00  30.00   47
  2  \w    -88.00  10.00   1.00   15.00    --  -18.53 -77.00 150.00   98
  3  \w    -89.00   4.00   1.00   15.00    --  -18.53 -37.00  60.00   93
  4  \w    -25.00  22.00   1.00   15.00    --  -18.53 -99.00 -90.00   47
  5  \w    -48.00  39.00   1.00   15.00    --   20.25 -57.00 -60.00   87
  6  \w    -48.00  39.00   1.00   15.00    --   20.25 -57.00-120.00   87
  7  \w    -48.00  39.00   1.00   15.00    --   20.25 -57.00   0.00   87
  8  \w    -93.00 -34.00   1.00   15.00    --  -18.53-179.00  30.00   59
  9  \w      2.00  89.00   1.00   15.00    --   20.25  57.00  30.00   87
 10  \w    -25.00  61.00   1.00   15.00    --   20.25 -99.00-180.00   86
 11  \w    -50.00  43.00   1.00   15.00    --   20.25 -37.00  30.00   93
 12  \w    -25.00  61.00   1.00   15.00    --   20.25 -99.00  30.00   86
 13  \w     -8.00  89.00   1.00   15.00    --   20.25  77.00 -60.00   97
 14  \w    -64.00  16.00   1.00   15.00    --  -18.53 109.00-160.00   80
 15  \w    -25.00  22.00   1.00   15.00    --  -18.53 -99.00-180.00   47
 16  \w    -87.00   0.00   1.00   15.00    --  -18.53 -57.00-150.00   87
 17  \w    -93.00 -34.00   1.00   15.00    --  -18.53-179.00  90.00   59
 18  \w    -25.00  57.00   1.00   15.00    --   20.25 -99.00 -60.00   82
 19  \w    -25.00  61.00   1.00   15.00    --   20.25 -99.00 150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0339838000
_diffrn_orient_matrix_UB_12      -0.0331077000
_diffrn_orient_matrix_UB_13      -0.0055909000
_diffrn_orient_matrix_UB_21      -0.0477094000
_diffrn_orient_matrix_UB_22      0.0183160000
_diffrn_orient_matrix_UB_23      -0.0289086000
_diffrn_orient_matrix_UB_31      0.0288811000
_diffrn_orient_matrix_UB_32      -0.0086775000
_diffrn_orient_matrix_UB_33      -0.0396942000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1614
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            85016
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       needle
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+1.7140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3757
_reflns_number_total             5866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           p17095_orth
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_database_code               7703025
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H100 Ce1 O5'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C242)=Sof(H24d)=Sof(H24e)=Sof(H24f)=Sof(C244)=Sof(H24j)=Sof(H24k)=
 Sof(H24l)=Sof(C246)=Sof(H24p)=Sof(H24q)=Sof(H24r)=1-FVAR(1)
 Sof(C241)=Sof(H24a)=Sof(H24b)=Sof(H24c)=Sof(C243)=Sof(H24g)=Sof(H24h)=
 Sof(H24i)=Sof(C245)=Sof(H24m)=Sof(H24n)=Sof(H24o)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C13(H13), C15(H15), C23(H23), C25(H25)
3.c Idealised Me refined as rotating group:
 C121(H12a,H12b,H12c), C122(H12d,H12e,H12f), C123(H12g,H12h,H12i), C141(H14a,
 H14b,H14c), C142(H14d,H14e,H14f), C143(H14g,H14h,H14i), C221(H22a,H22b,H22c),
 C222(H22d,H22e,H22f), C223(H22g,H22h,H22i), C241(H24a,H24b,H24c), C242(H24d,
 H24e,H24f), C243(H24g,H24h,H24i), C244(H24j,H24k,H24l), C245(H24m,H24n,H24o),
 C246(H24p,H24q,H24r)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.893
_oxdiff_exptl_absorpt_empirical_full_min 0.714