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_7703024
_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
'0.5(C124 H144 Ce2 K N4 O8), 0.25(C60 H60 K2 N12), 3(C5 H5 N), 0.5(C6 H14)'
_chemical_formula_sum            'C95 H109 Ce K N8 O4'
_chemical_formula_weight         1606.12
_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
_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                97.6409(9)
_cell_angle_beta                 103.4543(9)
_cell_angle_gamma                94.2363(6)
_cell_formula_units_Z            4
_cell_length_a                   17.29805(13)
_cell_length_b                   21.51193(16)
_cell_length_c                   25.0448(4)
_cell_measurement_reflns_used    73847
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.9930
_cell_measurement_theta_min      3.5060
_cell_volume                     8930.03(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega -114.00  -67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686 -134.0000  132.0000 47

  2 omega -122.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -19.0000  -90.0000 116

  3 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -120.0000 79

  4 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000   90.0000 79

  5 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -180.0000 79

  6 omega   29.00  103.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -134.0000  132.0000 74

  7 omega    1.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000 -180.0000 82

  8 omega   12.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686   77.0000  -60.0000 105

  9 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

 10 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 55

 11 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -90.0000 91

 12 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -90.0000 59

 13 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   60.0000 59

 14 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  150.0000 91

 15 omega   37.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   60.0000 105

 16 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -60.0000 91

 17 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 82

 18 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 82

 19 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 82

 20 omega   88.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   42.0000   53.6282 90

 21 omega   37.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -120.0000 105

 22 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 82

 23 omega   41.00  126.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -134.0000  132.0000 85

 24 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   64.0000  161.5391 95

 25 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -120.0000 98

 26 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 98

 27 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -150.0000 91

 28 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  150.0000 84

 29 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 79

 30 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 55

 31 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 91

 32 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 55

 33 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

 34 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 79

 35 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 82

 36 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000  120.0000 96

 37 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -180.0000 96

 38 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   30.0000 96

 39 omega    1.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000  -30.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0286758000
_diffrn_orient_matrix_UB_12      0.0280580000
_diffrn_orient_matrix_UB_13      0.0620549000
_diffrn_orient_matrix_UB_21      0.0174474000
_diffrn_orient_matrix_UB_22      0.0655280000
_diffrn_orient_matrix_UB_23      -0.0157245000
_diffrn_orient_matrix_UB_31      -0.0857859000
_diffrn_orient_matrix_UB_32      0.0142196000
_diffrn_orient_matrix_UB_33      0.0006793000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            181100
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.254
_diffrn_reflns_theta_min         3.509
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.762
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.195
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.4897
_exptl_crystal_size_mid          0.2254
_exptl_crystal_size_min          0.0328
_refine_diff_density_max         7.471
_refine_diff_density_min         -2.340
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1985
_refine_ls_number_reflns         37007
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1227P)^2^+33.7857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32721
_reflns_number_total             37007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           po16002_refinalized_fi
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_original_cell_volume        8930.03(16)
_cod_database_code               7703024
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C106 H134 Ce2 K O8'
_chemical_oxdiff_usercomment     '@ 120 K WK-K2L2Ce2-pyr'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C923-C924
 1.35 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N12, C935, C936, C937, C938, C939
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1(H1), C8(H8), C8A(H8A)
4.b Secondary CH2 refined with riding coordinates:
 C976(H97D,H97E), C977(H97F,H97G), C978(H97H,H97I), C979(H97J,H97K)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C4A(H4A), C4(H4), C6A(H6A), C6(H6), C7A(H7A), C7(H7),
 C13(H13), C0AA(H0AA), 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), C900(H900), C901(H901), C902(H902), C903(H903), C904(H904),
 C905(H905), C906(H906), C907(H907), C908(H908), C909(H909), C910(H910),
 C911(H911), C912(H912), C913(H913), C914(H914), C915(H915), C916(H916),
 C917(H917), C918(H918), C919(H919), C920(H920), C921(H921), C922(H922),
 C923(H923), C924(H924), C925(H925), C926(H926), C927(H927), C928(H928),
 C929(H929), C930(H930), C931(H931), C932(H932), C933(H933), C934(H934),
 C937(H937), C938(H938), C939(H939), C935(H935), C936(H936), C940(H940),
 C941(H941), C942(H942), C943(H943), C944(H944), C945(H945), C946(H946),
 C947(H947), C948(H948), C949(H949), C15(H15), C981(H981), C982(H982),
 C983(H983), C984(H984), C950(H950), C951(H951), C952(H952), C953(H953),
 C954(H954), C960(H960), C961(H961), C962(H962), C963(H963), C964(H964),
 C965(H965), C966(H966), C967(H967), C968(H968), C969(H969), C955(H955),
 C956(H956), C957(H957), C958(H958), C959(H959), C970(H970), C971(H971),
 C972(H972), C973(H973), C974(H974)
4.d Fitted hexagon refined as free rotating group:
 C937(C938,C939,N12,C935,C936)
4.e 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), C975(H97A,H97B,H97C), C980(H98A,H98B,H98C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'