The crystal structure of 1,1′-(((2 (dimethylamino)ethyl)azanediyl)bis(methylene)) bis(naphthalen-2-olato-κ4 N,N′,O,O′)-(pyridine-2,6-dicarboxylato-N,O,O′)- titanium(IV) ─ dichloromethane (2/1), C33H29N3O6Ti
Zhao, Tiankun; Wang, Peng; Ji, Mingyu; Li, Shanjia; Yang, Mingjun; Pu, Xiuying; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 985–987; doi:10.1515/ncrs-2021-0182

data_8104644
_publ_section_title
;
 The crystal structure of 1,1&#x2032;-(((2
 (dimethylamino)ethyl)azanediyl)bis(methylene)) bis(naphthalen-2-olato-\k4
 N,N&#x2032;,O,O&#x2032;)-(pyridine-2,6-dicarboxylato-N,O,O&#x2032;)-
 titanium(IV) &#x2500; dichloromethane (2/1), C33H29N3O6Ti
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              985
_journal_page_last               987
_journal_paper_doi               10.1515/ncrs-2021-0182
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C33 H29 N3 O6 Ti, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C33.5 H30 Cl N3 O6 Ti'
_chemical_formula_weight         653.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 116.009(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.4022(15)
_cell_length_b                   14.0345(7)
_cell_length_c                   17.0047(10)
_cell_measurement_reflns_used    9559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.09
_cell_measurement_theta_min      3.12
_cell_volume                     5877.3(6)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38312
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.089
_diffrn_reflns_theta_min         3.122
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.510
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00046(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0646P)^2^+4.0474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5177
_reflns_number_total             6027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0182_suppl.cif
_cod_data_source_block           210428d_0m
_cod_original_formula_sum        'C33.50 H30 Cl N3 O6 Ti'
_cod_database_code               8104644
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.753
_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. Others 
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) Cl1(0.5) Cl2(0.5) 
3.a Secondary CH2 refined with riding coordinates: 
 C11(H11A,H11B), C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C1S(H1SA,H1SB) 
3.b Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16), 
 C19(H19), C20(H20), C21(H21), C22(H22), C28(H28), C29(H29), C30(H30) 
3.c Idealised Me refined as rotating group: 
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C) 
;
_shelx_res_checksum              11372
_shelx_hkl_checksum              78769
_olex2_submission_special_instructions 'No special instructions were received'