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_7712174
_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         'C84 H72 Cu4 O16 Ti4'
_chemical_formula_sum            'C84 H72 Cu4 O16 Ti4'
_chemical_formula_weight         1783.17
_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             2022-12-17
_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                71.491(3)
_cell_angle_beta                 74.871(3)
_cell_angle_gamma                60.432(4)
_cell_formula_units_Z            2
_cell_length_a                   14.9176(6)
_cell_length_b                   15.1046(5)
_cell_length_c                   18.7494(6)
_cell_measurement_reflns_used    20642
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0080
_cell_measurement_theta_min      1.9320
_cell_volume                     3456.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.842
_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    -18.00  28.00   0.50    9.34    --   -5.15 -99.00  90.00   92
  2  \w    -79.00  10.00   0.50    9.34    --   -5.15 -38.00 150.00  178
  3  \w     -8.00  80.00   0.50    9.34    --    6.56  38.00  90.00  176
  4  \w    -18.00  40.00   0.50    9.34    --    6.56 -99.00 -30.00  116
  5  \w    -18.00  40.00   0.50    9.34    --    6.56 -99.00   0.00  116
  6  \w    -18.00  40.00   0.50    9.34    --    6.56 -99.00-180.00  116
  7  \w    -56.00  24.00   0.50    9.34    --    6.56 -77.00 -90.00  160
  8  \w    -14.00  73.00   0.50    9.34    --    6.56  77.00 150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0077195000
_diffrn_orient_matrix_UB_12      0.0235996000
_diffrn_orient_matrix_UB_13      -0.0388646000
_diffrn_orient_matrix_UB_21      0.0326600000
_diffrn_orient_matrix_UB_22      0.0160499000
_diffrn_orient_matrix_UB_23      0.0084954000
_diffrn_orient_matrix_UB_31      0.0437131000
_diffrn_orient_matrix_UB_32      -0.0474909000
_diffrn_orient_matrix_UB_33      -0.0058990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64963
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.501
_diffrn_reflns_theta_min         2.073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (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    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.042
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         17782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0876
_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^)+(0.1199P)^2^+18.0347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2232
_refine_ls_wR_factor_ref         0.2363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12796
_reflns_number_total             17782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03756d2.cif
_cod_data_source_block           dgg
_cod_depositor_comments
'Adding full bibliography for 7712172--7712174.cif.'
_cod_database_code               7712174
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C168  Cu8  O32  Ti8  '
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.627
_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 Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00Y(H00Y), C010(H010), C013(H013), C014(H014), C016(H016), C017(H017),
 C018(H018), C019(H019), C01C(H01C), C01G(H01G), C01H(H01H), C01I(H01I),
 C01L(H01L), C01M(H01M), C01S(H01S), C01T(H01T), C01U(H01U), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C022(H022), C024(H024), C026(H026), C02D(H02D),
 C02E(H02E), C02H(H02L), C02I(H02M), C02L(H02N), C02U(H02X), C02X(H02)
2.b Idealised Me refined as rotating group:
 C01J(H01A,H01B,H01D), C027(H02A,H02B,H02C), C02F(H02F,H02G,H02H), C02G(H02I,
 H02J,H02K), C02O(H02O,H02P,H02Q), C02P(H02R,H02S,H02T), C02R(H02U,H02V,H02W),
 C02V(H02Y,H,HA), C02W(H02Z,HB,HC), C02Y(H1,HD,HE), C02Z(H2,HF,HG), C030(H03A,
 H03B,H03C)
;
_shelx_res_checksum              16289
_shelx_hkl_checksum              84260
_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 1.503
_oxdiff_exptl_absorpt_empirical_full_min 0.627