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_7701737
_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         'C29 H57 N7 O8 Ti3'
_chemical_formula_sum            'C29 H57 N7 O8 Ti3'
_chemical_formula_weight         775.51
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-05
_audit_creation_method
;
Olex2 1.2
(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                90
_cell_angle_beta                 98.629(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7979(6)
_cell_length_b                   23.8477(14)
_cell_length_c                   13.0520(7)
_cell_measurement_reflns_used    3626
_cell_measurement_temperature    100.00(15)
_cell_measurement_theta_max      70.0660
_cell_measurement_theta_min      4.8980
_cell_volume                     3938.4(4)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.937
_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    -19.00  42.00   1.00    1.00    --    0.00  38.00  30.00   61
  2  \w    -18.00  52.00   1.00    1.00    --    0.00  57.00-120.00   70
  3  \w     -2.00  64.00   1.00    1.00    --   54.00 -77.00-180.00   66
  4  \w     12.00  96.00   1.00    1.00    --   54.00 -99.00 -60.00   84
  5  \w    -16.00  84.00   1.00    1.00    --   54.00 -77.00  60.00  100
  6  \w     58.00  93.00   1.00    1.00    --   54.00  57.00-120.00   35
  7  \w     40.00 122.00   1.00    1.00    --  108.00 -63.00  60.00   82
  8  \w    133.00 162.00   1.00    1.00    --  108.00  50.00 -30.00   29
  9  \w     43.00 112.00   1.00    1.00    --  108.00-111.00 -60.00   69
 10  \w     93.00 172.00   1.00    1.00    --  108.00  50.00  30.00   79
 11  \w     38.00  68.00   1.00    1.00    --  108.00 -77.00-120.00   30
 12  \w     91.00 176.00   1.00    1.00    --  108.00  63.00 120.00   85
 13  \w     67.00 128.00   1.00    1.00    --  108.00 -63.00 -90.00   61
 14  \w     36.00 102.00   1.00    1.00    --  108.00-111.00-120.00   66
 15  \w     93.00 141.00   1.00    1.00    --  108.00  38.00  90.00   48
 16  \w     69.00 118.00   1.00    1.00    --  108.00 -77.00   0.00   49
;
_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      -0.0545242000
_diffrn_orient_matrix_UB_12      0.0042622000
_diffrn_orient_matrix_UB_13      0.0971992000
_diffrn_orient_matrix_UB_21      -0.0430261000
_diffrn_orient_matrix_UB_22      0.0583209000
_diffrn_orient_matrix_UB_23      -0.0352743000
_diffrn_orient_matrix_UB_31      -0.0999941000
_diffrn_orient_matrix_UB_32      -0.0274994000
_diffrn_orient_matrix_UB_33      -0.0596291000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16294
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.960
_diffrn_reflns_theta_min         3.895
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01965
_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            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+0.8790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4915
_reflns_number_total             7129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01628g2.cif
_cod_data_source_block           PTC-196
_cod_database_code               7701737
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         COTi
_reflns_odcompleteness_completeness 95.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C9(H9), C17(H17), C5(H5), C13(H13), C34(H34), C21(H21), C30(H30)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C26(H26), C47(H47), C42(H42), C28(H28), C45(H45), C40(H40), C41(H41)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C35(H35A,H35B,H35C), C6(H6A,H6B,
 H6C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,
 H31B,H31C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C15(H15A,H15B,H15C),
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              8589
_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 16.979
_oxdiff_exptl_absorpt_empirical_full_min 0.311