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_7703019
_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 Cl N4 O2 Pr, 2(C5 H5 N)'
_chemical_formula_sum            'C62 H73 Cl N6 O2 Pr'
_chemical_formula_weight         1110.62
_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             2019-07-09
_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                76.5680(10)
_cell_angle_beta                 80.439(2)
_cell_angle_gamma                62.616(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8885(3)
_cell_length_b                   14.0584(2)
_cell_length_c                   20.1573(3)
_cell_measurement_reflns_used    16893
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4960
_cell_measurement_theta_min      3.3740
_cell_volume                     3391.09(12)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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 0.905
_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   22.50    --  -18.68 -99.00 -60.00   47
  2  \w    -25.00  22.00   1.00   22.50    --  -18.68 -99.00 150.00   47
  3  \w     34.00  95.00   1.00   22.50    --   20.40 179.00 -30.00   61
  4  \w     34.00  95.00   1.00   22.50    --   20.40 179.00  30.00   61
  5  \w    -48.00  39.00   1.00   22.50    --   20.40 -57.00   0.00   87
  6  \w    -48.00  39.00   1.00   22.50    --   20.40 -57.00  60.00   87
  7  \w     32.00  95.00   1.00   22.50    --   20.40-179.00 150.00   63
  8  \w    -48.00  39.00   1.00   22.50    --   20.40 -57.00  30.00   87
  9  \w     -2.00  91.00   1.00   22.50    --   20.40  38.00-180.00   93
 10  \w    -87.00   0.00   1.00   22.50    --  -18.68 -57.00-120.00   87
 11  \w    -37.00  50.00   1.00   22.50    --  -18.68  57.00 150.00   87
 12  \w      2.00  27.00   1.00   22.50    --   20.40  57.00  30.00   25
 13  \w      1.00  80.00   1.00   22.50    --   20.40-132.00-151.00   79
 14  \w    -25.00  61.00   1.00   22.50    --   20.40 -99.00 -90.00   86
 15  \w      2.00  89.00   1.00   22.50    --   20.40  57.00  60.00   87
;
_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      -0.0242998000
_diffrn_orient_matrix_UB_12      0.0553992000
_diffrn_orient_matrix_UB_13      -0.0161193000
_diffrn_orient_matrix_UB_21      0.0174977000
_diffrn_orient_matrix_UB_22      -0.0159478000
_diffrn_orient_matrix_UB_23      -0.0324769000
_diffrn_orient_matrix_UB_31      -0.0492655000
_diffrn_orient_matrix_UB_32      -0.0033032000
_diffrn_orient_matrix_UB_33      -0.0006732000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.286
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89721
_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 light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         18379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+1.5959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14510
_reflns_number_total             18379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03291f2.cif
_cod_data_source_block           p16195
_cod_depositor_comments
'Adding full bibliography for 7703018--7703028.cif.'
_cod_database_code               7703019
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C70 H70 O4 Pr2 Cl2 N8'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C13(H13), C15(H15), C23(H23), C25(H25), 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)
2.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)
;
_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 1.168
_oxdiff_exptl_absorpt_empirical_full_min 0.858