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_7701735
_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         'C24 H30 N4 O7 Ti2, C3 H4 N2'
_chemical_formula_sum            'C26 H34 N7 O7 Ti2'
_chemical_formula_weight         652.40
_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             2019-05-06
_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                101.117(4)
_cell_angle_beta                 96.655(8)
_cell_angle_gamma                98.380(5)
_cell_formula_units_Z            2
_cell_length_a                   11.235(5)
_cell_length_b                   11.733(5)
_cell_length_c                   12.526(6)
_cell_measurement_reflns_used    4612
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5087
_cell_measurement_theta_min      3.3521
_cell_volume                     1585.2(12)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12496
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         3.352
_exptl_absorpt_coefficient_mu    0.556
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       Prism
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6842
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1370P)^2^+0.1244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5454
_reflns_number_total             6842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01628g2.cif
_cod_data_source_block           PTC-195
_cod_original_cell_volume        1585.3(12)
_cod_database_code               7701735
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H00E-H00Z
 2 with sigma of 0.02
 H00F-H00Z
 2 with sigma of 0.02
3.a :
 N00Y(N010,C4,C5,C6)
3.b Ternary CH refined with riding coordinates:
 C00Z(H00Z), C012(H012)
3.c Aromatic/amide H refined with riding coordinates:
 N00A(H00A), N00B(H00B), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), N00Y(H00Y), C4(H4), C5(H5),
 C6(H6)
3.d Idealised Me refined as rotating group:
 C00W(H00C,H00D,H00E), C00X(H00F,H00G,H00O), C011(H01A,H01B,H01C), C013(H01D,
 H01E,H01F)
;
_shelx_res_checksum              40695
_olex2_submission_special_instructions 'No special instructions were received'