Pyrazole-thermal synthesis: a new approach towards N-rich titanium-oxo clusters with photochromic behaviors.
Fan, Xi; Fu, Hao; Zhang, Lei; Zhang, Jian; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8049–8052; doi:10.1039/c9dt01628g

data_7701736
_publ_section_title
;
 Pyrazole-thermal synthesis: a new approach towards N-rich titanium-oxo
 clusters with photochromic behaviors.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8049
_journal_page_last               8052
_journal_paper_doi               10.1039/c9dt01628g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H96 N24 O20 Ti10'
_chemical_formula_sum            'C60 H96 N24 O20 Ti10'
_chemical_formula_weight         1952.60
_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             2018-06-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-06 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                93.789(2)
_cell_angle_beta                 99.033(2)
_cell_angle_gamma                104.107(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7282(4)
_cell_length_b                   14.6322(3)
_cell_length_c                   23.1079(6)
_cell_measurement_reflns_used    14108
_cell_measurement_temperature    295.56(10)
_cell_measurement_theta_max      70.4040
_cell_measurement_theta_min      4.5390
_cell_volume                     4419.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      air
_diffrn_ambient_temperature      295.56(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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    -20.00  30.00   1.00    1.00    --    0.00  57.00  30.00   50
  2  \w     44.00  69.00   1.00    1.00    --    0.00  57.00  30.00   25
  3  \w    -23.00   7.00   1.00    1.00    --    0.00 112.00  63.00   30
  4  \w    -13.00  20.00   1.00    1.00    --    0.00 -57.00-120.00   33
  5  \w    -67.00 -15.00   1.00    1.00    --    0.00 -57.00-120.00   52
  6  \w     10.00 127.00   1.00    1.16    --   54.00  19.00 -90.00  117
  7  \w      3.00  29.00   1.00    1.16    --   54.00 -57.00 150.00   26
  8  \w     38.00  65.00   1.00    1.16    --   54.00-125.00-180.00   27
  9  \w    -14.00  74.00   1.00    1.16    --   54.00 -57.00 -90.00   88
 10  \w    -15.00  69.00   1.00    1.16    --   54.00 -57.00   0.00   84
 11  \w     84.00 109.00   1.00    1.16    --   54.00-125.00-180.00   25
 12  \w     36.00 103.00   1.00    1.16    --   54.00-125.00 -90.00   67
 13  \w     25.00 120.00   1.00    1.16    --   54.00  77.00 120.00   95
 14  \w    112.00 137.00   1.00    1.16    --  108.00 111.00-150.00   25
 15  \w     60.00 107.00   1.00    1.16    --  108.00-111.00 120.00   47
 16  \w     50.00 126.00   1.00    1.16    --  108.00 -50.00  30.00   76
 17  \w    110.00 146.00   1.00    1.16    --  108.00 112.00  63.00   36
 18  \w     90.00 152.00   1.00    1.16    --  108.00  63.00  60.00   62
 19  \w     52.00 137.00   1.00    1.16    --  108.00 -77.00 120.00   85
 20  \w     87.00 113.00   1.00    1.16    --  108.00-111.00-150.00   26
 21  \w     77.00 109.00   1.00    1.16    --  108.00-111.00  60.00   32
 22  \w     37.00 109.00   1.00    1.16    --  108.00-111.00 -60.00   72
 23  \w     36.00 134.00   1.00    1.16    --  108.00 -38.00 120.00   98
 24  \w    102.00 127.00   1.00    1.16    --  108.00 111.00  90.00   25
 25  \w    100.00 126.00   1.00    1.16    --  108.00 111.00   0.00   26
 26  \w     40.00 134.00   1.00    1.16    --  108.00 -38.00 -90.00   94
 27  \w     42.00 178.00   1.00    1.16    --  108.00  12.00-180.00  136
 28  \w     41.00 134.00   1.00    1.16    --  108.00 -77.00 -60.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0569024000
_diffrn_orient_matrix_UB_12      -0.0323539000
_diffrn_orient_matrix_UB_13      -0.0637940000
_diffrn_orient_matrix_UB_21      0.1007938000
_diffrn_orient_matrix_UB_22      -0.0069088000
_diffrn_orient_matrix_UB_23      -0.0190855000
_diffrn_orient_matrix_UB_31      -0.0208225000
_diffrn_orient_matrix_UB_32      -0.1040776000
_diffrn_orient_matrix_UB_33      0.0133345000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31097
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.506
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.455
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         16568
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.5875P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13921
_reflns_number_total             16568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01628g2.cif
_cod_data_source_block           PTC-197
_cod_database_code               7701736
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         CONTi
_chemical_oxdiff_usercomment     fx15-21-20
_reflns_odcompleteness_completeness 99.94
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(H1B)=Sof(C3A)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=1-FVAR(1)
 Sof(H1A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C01W(H01W), C01Z(H01Z), C021(H021), C02E(H02E), C02P(H02T), C02R(H02X),
 C030(H030), C1(H1A), C1(H1B)
4.b Aromatic/amide H refined with riding coordinates:
 N01E(H01E), N01F(H01F), N01G(H01G), N01I(H01I), C01J(H01J), C01K(H01K),
 C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q),
 C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01X(H01X),
 C01Y(H01Y), C020(H020), C022(H022), C023(H023), C024(H024), C025(H025),
 C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A), C02B(H02B),
 C02C(H02C), C02D(H02D), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I),
 C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M)
4.c Idealised Me refined as rotating group:
 C02N(H02N,H02O,H02P), C02O(H02Q,H02R,H02S), C02Q(H02U,H02V,H02W), C02S(H02Y,H,
 HA), C02T(H02Z,HB,HC), C02U(H02,HD,HE), C02V(H0AA,HF,HG), C02W(H1AA,HH,HI),
 C02X(H2AA,HJ,HK), C02Y(H3AA,HL,HM), C02Z(H4AA,HN,HO), C031(H03A,H03B,H03C),
 C033(H03D,H03E,H03F), C034(H03G,H03H,H03I), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C),
 C3A(H3AB,H3AC,H3AD), C9A(H9AA,H9AB,H9AC)
;
_shelx_res_checksum              39818
_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 3.475
_oxdiff_exptl_absorpt_empirical_full_min 0.638