The crystal structure of 6,6′-(((2-(dimethylamino)ethyl)azanediyl)bis(methylene))bis(2-chloro-4-methyl phenolate-κ 4 N,N′,O,O′)-(pyridine-2,6-dicarboxylato-N,O,O′)-titanium(IV), C27H27Cl2N3O6Ti
Yang, Mingjun; Wang, Canghai; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 817–819; doi:10.1515/ncrs-2023-0168

data_8107572
_publ_section_title
;
 The crystal structure of
 6,6&#x2032;-(((2-(dimethylamino)ethyl)azanediyl)bis(methylene))bis(2-chloro-4-methyl
 phenolate-\k 4
 N,N&#x2032;,O,O&#x2032;)-(pyridine-2,6-dicarboxylato-N,O,O&#x2032;)-titanium(IV),
 C27H27Cl2N3O6Ti
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              817
_journal_page_last               819
_journal_paper_doi               10.1515/ncrs-2023-0168
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C27 H27 Cl2 N3 O6 Ti'
_chemical_formula_sum            'C27 H27 Cl2 N3 O6 Ti'
_chemical_formula_weight         608.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 109.881(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.609(4)
_cell_length_b                   21.476(7)
_cell_length_c                   13.504(4)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      59.45
_cell_measurement_theta_min      3.03
_cell_volume                     3166.1(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XM  (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23033
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.995
_diffrn_reflns_theta_min         3.518
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.808
_exptl_absorpt_correction_T_max  0.7520
_exptl_absorpt_correction_T_min  0.2606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4698
_reflns_number_total             6002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0168_suppl_001.cif
_cod_data_source_block           a_0m
_cod_original_cell_volume        3166.2(18)
_cod_database_code               8107572
_shelx_estimated_absorpt_t_max   0.604
_shelx_estimated_absorpt_t_min   0.486
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Secondary CH2 refined with riding coordinates: 
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B) 
2.b Aromatic/amide H refined with riding coordinates: 
 C3(H3), C5(H5), C13(H13), C15(H15), C22(H22), C23(H23), C24(H24) 
2.c Idealised Me refined as rotating group: 
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C) 
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92153
_shelx_hkl_checksum              93178
_shelx_fab_checksum              46226
_olex2_submission_special_instructions 'No special instructions were received'