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_7703018
_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         'C148 H212 K8 O19'
_chemical_formula_sum            'C148 H212 K8 O19'
_chemical_formula_weight         2607.96
_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   geom
_atom_sites_solution_primary     direct
_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                 97.896(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9449(7)
_cell_length_b                   27.0456(9)
_cell_length_c                   25.5786(8)
_cell_measurement_reflns_used    18394
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.5230
_cell_measurement_theta_min      2.9980
_cell_volume                     15722.5(9)
_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      170(2)
_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 0.998
_diffrn_measurement_details
;
  1 omega  -25.00   26.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694  -99.0000  -30.0000 51

  2 omega  -25.00   26.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694  -99.0000 -180.0000 51

  3 omega  -88.00  -34.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694 -179.0000 -180.0000 54

  4 omega  -88.00  -34.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694 -179.0000 -120.0000 54

  5 omega  -83.00    4.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694  -57.0000  -90.0000 87

  6 omega  -88.00  -34.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694 -179.0000  -60.0000 54

  7 omega  -83.00    4.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694  -57.0000  150.0000 87

  8 omega  -37.00   56.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694   38.0000 -150.0000 93

  9 omega  -43.00   55.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694   77.0000 -120.0000 98

 10 omega  -83.00    4.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2694  -57.0000   60.0000 87

 11 omega   34.00   82.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       15.9881  179.0000 -150.0000 48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0292463000
_diffrn_orient_matrix_UB_12      0.0088298000
_diffrn_orient_matrix_UB_13      -0.0012062000
_diffrn_orient_matrix_UB_21      -0.0107460000
_diffrn_orient_matrix_UB_22      -0.0245135000
_diffrn_orient_matrix_UB_23      -0.0038357000
_diffrn_orient_matrix_UB_31      0.0015771000
_diffrn_orient_matrix_UB_32      -0.0029963000
_diffrn_orient_matrix_UB_33      0.0277154000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1376
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            205920
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.846
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.937
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.7994
_exptl_crystal_size_mid          0.5264
_exptl_crystal_size_min          0.1778
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1608
_refine_ls_number_reflns         24952
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.0942
_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^)+(0.1197P)^2^+23.9256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12916
_reflns_number_total             24952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           p16039_monoclinic
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_database_code               7703018
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 O4 K4'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.809
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_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
 O10, C904, C905, C906, C907
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C8A(H8A), C8(H8)
3.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), C916(H91M,H91N), C917(H91O,H91P),
 C918(H91Q,H91R), C919(H91S,H91T), C920(H92A,H92B), C921(H92C,H92D), C922(H92E,
 H92F), C923(H92G,H92H), C928(H92I,H92J), C929(H92K,H92L), C930(H93A,H93B),
 C931(H93C,H93D), C932(H93E,H93F), C933(H93G,H93H), C934(H93I,H93J), C935(H93K,
 H93L), C936(H93M,H93N), C937(H93O,H93P), C938(H93Q,H93R), C939(H93S,H93T),
 C940(H94A,H94B), C941(H94C,H94D), C942(H94E,H94F), C943(H94G,H94H), C944(H94I,
 H94J), C945(H94K,H94L), C946(H94M,H94N), C947(H94O,H94P)
3.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3(H3), C4(H4), C4A(H4A), C6A(H6A), C6(H6), 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), C83(H83), C85(H85)
3.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,
 H12H,H12I), C140(H14A,H14B,H14C), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F),
 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'