An anionic η<sup>2</sup>-naphthalene complex of titanium supported by a tripodal [O<sub>3</sub>C] ligand and its reactions with dinitrogen, anthracene and THF.
Nakanishi, Yusuke; Ishida, Yutaka; Kawaguchi, Hiroyuki; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6903–6907; doi:10.1039/c8dt01161c

data_7046234
_publ_section_title
;
 An anionic \h<sup>2</sup>-naphthalene complex of titanium supported by a
 tripodal [O<sub>3</sub>C] ligand and its reactions with dinitrogen,
 anthracene and THF.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6903
_journal_page_last               6907
_journal_paper_doi               10.1039/c8dt01161c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C61 H80 K O5 Ti, C16 H40 K O8, C61 H77.8 K O5 Ti, C12 H30 K O6'
_chemical_formula_sum            'C150 H230 K4 O24 Ti2'
_chemical_formula_weight         2669.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-03-14 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.267(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2683(8)
_cell_length_b                   20.1451(8)
_cell_length_c                   20.8247(9)
_cell_measurement_reflns_used    22932
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.8850
_cell_measurement_theta_min      3.0860
_cell_volume                     7516.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -110.00  70.00   0.50   32.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   32.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50   32.00    --  -20.00  45.00 180.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0228329000
_diffrn_orient_matrix_UB_12      0.0156693000
_diffrn_orient_matrix_UB_13      -0.0194224000
_diffrn_orient_matrix_UB_21      0.0203718000
_diffrn_orient_matrix_UB_22      -0.0299085000
_diffrn_orient_matrix_UB_23      -0.0005364000
_diffrn_orient_matrix_UB_31      -0.0251241000
_diffrn_orient_matrix_UB_32      -0.0099838000
_diffrn_orient_matrix_UB_33      -0.0287838000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.1689
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91218
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       needle
_exptl_crystal_F_000             2884
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1787
_refine_ls_number_reflns         33702
_refine_ls_number_restraints     2007
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.0742
_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^)+(0.0680P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                19280
_reflns_number_total             33702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01161c2.cif
_cod_data_source_block           o3ctianth_3rd_dme
_cod_depositor_comments
'Adding full bibliography for 7046232--7046237.cif.'
_cod_database_code               7046234
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.115
_oxdiff_exptl_absorpt_empirical_full_min 0.945