Cu<sub>4</sub>Ti<sub>4</sub>-oxo clusters functionalized by <i>in situ</i> - generated 2,2'-biphenolate ligands from the oxidative coupling of phenols.
Liu, Xiao-Xue; Wang, Zi-Rui; Chen, Guang-Hui; Li, Qiao-Hong; Tao, Jun; Zhang, Lei; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1857–1860; doi:10.1039/d2dt03756d

data_7712172
_publ_section_title
;
 Cu<sub>4</sub>Ti<sub>4</sub>-oxo clusters functionalized by <i>in
 situ</i> - generated 2,2'-biphenolate ligands from the oxidative coupling
 of phenols.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1857
_journal_page_last               1860
_journal_paper_doi               10.1039/d2dt03756d
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C72 H48 Cu4 O16 Ti4, 4(C6 H6 O), 0.5[C6H5OH], 1[C6H5OH]'
_chemical_formula_sum            'C105 H81 Cu4 O21.5 Ti4'
_chemical_formula_weight         2132.45
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-22 deposited with the CCDC.	2022-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0478(2)
_cell_length_b                   27.1305(2)
_cell_length_c                   21.1066(2)
_cell_measurement_reflns_used    31700
_cell_measurement_temperature    100.00(18)
_cell_measurement_theta_max      75.1070
_cell_measurement_theta_min      2.5810
_cell_volume                     8606.53(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -130.00  47.00   1.00    1.46    --  -41.54   0.00  60.00  177
  2  \w     27.00  98.00   1.00    1.46    --   41.54-125.00 -60.00   71
  3  \w     27.00  98.00   1.00    1.46    --   41.54-125.00-180.00   71
  4  \w    104.00 178.00   1.00   10.00    --  108.23 111.00  30.00   74
  5  \w    103.00 178.00   1.00   10.00    --  108.23  77.00  60.00   75
  6  \w     32.00 141.00   1.00   10.00    --  108.23 -77.00  90.00  109
  7  \w     26.00 106.00   1.00   10.00    --  108.23 -94.00   0.00   80
  8  \w     61.00 146.00   1.00   10.00    --  108.23 178.00  90.00   85
  9  \w    103.00 172.00   1.00   10.00    --  108.23  77.00  90.00   69
 10  \w    149.00 178.00   1.00   10.00    --  108.23 111.00-180.00   29
 11  \w     81.00 177.00   1.00   10.00    --  108.23  61.00-150.00   96
 12  \w    135.00 170.00   1.00   10.00    --  108.23 111.00  60.00   35
 13  \w     60.00 107.00   1.00   10.00    --  108.23-111.00-180.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49506
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.654
_exptl_absorpt_coefficient_mu    4.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             4348
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.845
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.092
_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     1117
_refine_ls_number_reflns         15149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+19.0828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12820
_reflns_number_total             15149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03756d2.cif
_cod_data_source_block           ptc-331
_cod_depositor_comments
'Adding full bibliography for 7712172--7712174.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C105 H81 Cu4 O21.50 Ti4'
_cod_database_code               7712172
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Riding coordinates:
 O19(H19), O20(H20A), O17(H17A), O18(H18)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C69(H69), C59(H59), C49(H49), C72(H72), C61(H61), C6(H6), C64(H64),
 C14(H14), C70(H70), C26(H26), C35(H35), C38(H38), C47(H47), C73(H73), C23(H23),
  C77(H77), C71(H71), C41(H41), C12(H12), C92(H92), C3(H3), C29(H29), C10(H10),
 C58(H58), C65(H65), C52(H52), C50(H50), C20(H20), C27(H27), C66(H66), C28(H28),
  C32(H32), C57(H57), C56(H56), C34(H34), C93(H93), C11(H11), C39(H39),
 C46(H46), C33(H33), C17(H17), C45(H45), C16(H16), C76(H76), C44(H44), C21(H21),
  C15(H15), C22(H22), C51(H51), C5(H5), C40(H40), C96(H96), C4(H4), C74(H74),
 C75(H75), C94(H94), C95(H95), C80(H80), C86(H86), C84(H84), C90(H90), C83(H83),
  C87(H87), C89(H89), C88(H88), C81(H81), C82(H82)
;
_shelx_res_checksum              92674
_shelx_hkl_checksum              70220
_shelx_fab_checksum              30763
_platon_squeeze_void_probe_radius 1.20
_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
;