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_7703026
_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
'C144 H204 K O12 Pr2, C24 H48 K O6, 3(C4 H8 O)'
_chemical_formula_sum            'C180 H276 K2 O21 Pr2'
_chemical_formula_weight         3136.01
_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     dual
_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                 101.184(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6073(7)
_cell_length_b                   31.2563(11)
_cell_length_c                   33.684(2)
_cell_measurement_reflns_used    9504
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      67.7920
_cell_measurement_theta_min      3.5260
_cell_volume                     19218.4(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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   -113.00 -17.00   1.00   15.00    --  -43.17 -57.00 -60.00   96
  2  \w   -116.00 -21.00   1.00   15.00    --  -43.17 -38.00 150.00   95
  3  \w    -96.00  -2.00   1.00   15.00    --  -43.17 125.00  60.00   94
  4  \w    -70.00  27.00   1.00   15.00    --  -43.17  57.00 -60.00   97
  5  \w   -113.00 -17.00   1.00   15.00    --  -43.17 -57.00  30.00   96
  6  \w     23.00  98.00   1.00   15.00    --   43.17-125.00 -30.00   75
  7  \w     39.00 121.00   1.00   30.00    --  111.00-125.00 -60.00   82
  8  \w     36.00 135.00   1.00   30.00    --  111.00 -30.00 120.00   99
  9  \w     36.00 135.00   1.00   30.00    --  111.00 -30.00-120.00   99
 10  \w     41.00 139.00   1.00   30.00    --  111.00 -61.00-180.00   98
 11  \w     48.00  73.00   1.00   30.00    --  111.00-125.00 150.00   25
 12  \w     89.00 121.00   1.00   30.00    --  111.00-125.00 150.00   32
 13  \w    116.00 154.00   1.00   30.00    --  111.00 -15.00 -90.00   38
 14  \w     92.00 161.00   1.00   30.00    --  111.00  15.00-150.00   69
 15  \w     80.00 107.00   1.00   30.00    --  111.00 -94.00  30.00   27
 16  \w     47.00 129.00   1.00   30.00    --  111.00 -30.00 -30.00   82
 17  \w     30.00 108.00   1.00   30.00    --  111.00 -94.00-180.00   78
 18  \w     58.00 108.00   1.00   30.00    --  111.00 -94.00 120.00   50
 19  \w     64.00 121.00   1.00   30.00    --  111.00-125.00   0.00   57
 20  \w     89.00 176.00   1.00   30.00    --  111.00  15.00 150.00   87
 21  \w     30.00  65.00   1.00   30.00    --  111.00 -94.00  30.00   35
 22  \w    112.00 138.00   1.00   30.00    --  111.00 -77.00 -30.00   26
 23  \w     56.00 109.00   1.00   30.00    --  111.00 -94.00   0.00   53
 24  \w     77.00 137.00   1.00   30.00    --  111.00 -61.00 -30.00   60
 25  \w     32.00  89.00   1.00   30.00    --  111.00 -15.00 -90.00   57
 26  \w     82.00 110.00   1.00   30.00    --  111.00  77.00 -90.00   28
 27  \w     75.00 121.00   1.00   30.00    --  111.00-125.00-120.00   46
 28  \w     39.00 141.00   1.00   30.00    --  111.00 -77.00-120.00  102
 29  \w    116.00 145.00   1.00   30.00    --  111.00  30.00-120.00   29
 30  \w     38.00  64.00   1.00   30.00    --  111.00 -77.00 -30.00   26
 31  \w     87.00 148.00   1.00   30.00    --  111.00  30.00 -60.00   61
 32  \w    143.00 178.00   1.00   30.00    --  111.00  77.00 -90.00   35
 33  \w     77.00 104.00   1.00   30.00    --  111.00 -94.00 -30.00   27
 34  \w    110.00 135.00   1.00   30.00    --  111.00 -77.00 120.00   25
 35  \w     40.00  83.00   1.00   30.00    --  111.00 -77.00 120.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0357636000
_diffrn_orient_matrix_UB_12      -0.0071843000
_diffrn_orient_matrix_UB_13      0.0447223000
_diffrn_orient_matrix_UB_21      0.0763996000
_diffrn_orient_matrix_UB_22      0.0018983000
_diffrn_orient_matrix_UB_23      -0.0111702000
_diffrn_orient_matrix_UB_31      0.0022792000
_diffrn_orient_matrix_UB_32      0.0487223000
_diffrn_orient_matrix_UB_33      0.0070039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2725
_diffrn_reflns_av_unetI/netI     0.1480
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            238347
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.128
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43h (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    1.084
_exptl_crystal_description       plate
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.523
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.000060(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1895
_refine_ls_number_reflns         34807
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1678
_refine_ls_R_factor_gt           0.1068
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1664P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2719
_refine_ls_wR_factor_ref         0.3281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18518
_reflns_number_total             34807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           po16012_reint_0p83a
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_original_cell_volume        19218.7(15)
_cod_database_code               7703026
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C106 H134 Pr2 K O8'
_chemical_oxdiff_usercomment     '@ 120 K WK-575'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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
 C441, C440, C442, C443
 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), C924(H92I,H92J), C925(H92K,H92L), C926(H92M,H92N),
 C927(H92O,H92P), C928(H92Q,H92R), C929(H92S,H92T), 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), C941(H94A,
 H94B), C940(H94C,H94D), C942(H94E,H94F), C943(H94G,H94H), C944(H94I,H94J),
 C945(H94K,H94L), C946(H94M,H94N), C947(H94O,H94P), C948(H94Q,H94R), C949(H94S,
 H94T), C950(H95A,H95B), C951(H95C,H95D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C4(H4), C4A(H4A), C6A(H6A), C6(H6), C7A(H7A), C7(H7),
 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:
 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), C321(H32A,H32B,H32C), C322(H32D,H32E,H32F),
 C323(H32G,H32H,H32I), C341(H34A,H34B,H34C), C342(H34D,H34E,H34F), C343(H34G,
 H34H,H34I), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F), C423(H42G,H42H,H42I),
 C441(H44A,H44B,H44C), C442(H44D,H44E,H44F), C443(H44G,H44H,H44I), C521(H52A,
 H52B,H52C), C522(H52D,H52E,H52F), C523(H52G,H52H,H52I), C541(H54A,H54B,H54C),
 C542(H54D,H54E,H54F), C543(H54G,H54H,H54I), C621(H62A,H62B,H62C), C622(H62D,
 H62E,H62F), C623(H62G,H62H,H62I), C641(H64A,H64B,H64C), C642(H64D,H64E,H64F),
 C643(H64G,H64H,H64I), C721(H72A,H72B,H72C), C722(H72D,H72E,H72F), C723(H72G,
 H72H,H72I), C741(H74A,H74B,H74C), C742(H74D,H74E,H74F), C743(H74G,H74H,H74I),
 C821(H82A,H82B,H82C), C822(H82D,H82E,H82F), C823(H82G,H82H,H82I), C841(H84A,
 H84B,H84C), C842(H84D,H84E,H84F), C843(H84G,H84H,H84I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.673