The crystal structure of 6,6′-(((2-(dimethylamino)ethyl)azanediyl)bis(methylene))bis(benzo[d][1,3]dioxol-5-ol ato-κ4 N,N′,O,O′)-(pyridine-2,6-dicarboxylato-N,O,O′)-titanium(IV)-dichloromethane(1/1), C27H25N3O10Ti
Li, Shanjia; Wang, Peng; Ji, Mingyu; Yang, Mingjun; Pu, Xiuying; Zhao, Tiankun; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1165–1167; doi:10.1515/ncrs-2021-0260

data_8104556
_publ_section_title
;
 The crystal structure of
 6,6&#x2032;-(((2-(dimethylamino)ethyl)azanediyl)bis(methylene))bis(benzo[d][1,3]dioxol-5-ol
 ato-\k4
 N,N&#x2032;,O,O&#x2032;)-(pyridine-2,6-dicarboxylato-N,O,O&#x2032;)-titanium(IV)-dichloromethane(1/1),
 C27H25N3O10Ti
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1165
_journal_page_last               1167
_journal_paper_doi               10.1515/ncrs-2021-0260
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C27 H25 N3 O10 Ti, C H2 Cl2'
_chemical_formula_sum            'C28 H27 Cl2 N3 O10 Ti'
_chemical_formula_weight         684.32
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.839(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3366(11)
_cell_length_b                   11.0253(11)
_cell_length_c                   23.716(2)
_cell_measurement_reflns_used    1785
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.049
_cell_measurement_theta_min      2.171
_cell_volume                     2911.4(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_unetI/netI     0.1481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15865
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.749
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_meas      .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5125
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1596
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2257
_reflns_number_total             5125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0260_suppl.cif
_cod_data_source_block           mo_210526a_0m
_cod_database_code               8104556
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C18-N2 \\sim C18A-N2
 with sigma of 0.02
 C19-N2 \\sim C19A-N2
 with sigma of 0.02
 C20-N2 \\sim C20A-N2
 with sigma of 0.02
 C28-Cl1 \\sim C28A-Cl1A
 with sigma of 0.02
 C28-Cl2 \\sim C28A-Cl2A
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C19A) = Uanis(C19)
Uanis(Cl2) = Uanis(Cl2A)
Uanis(Cl1) = Uanis(Cl1A)
Uanis(C28) = Uanis(C28A)
4. Others
 Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(Cl1A)=Sof(Cl2A)=1-FVAR(2)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(Cl1)=Sof(Cl2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C16(H16A,H16B), C17(H17A,H17B),
 C17(H17C,H17D), C18(H18A,H18B), C18A(H18C,H18D), C28(H28A,H28B), C28A(H28C,
 H28D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C12(H12), C15(H15), C22(H22), C23(H23), C24(H24)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,H20C), C20A(H20D,
 H20E,H20F)
;
_shelx_res_checksum              74084
_shelx_hkl_checksum              43585
_olex2_submission_special_instructions 'No special instructions were received'