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_7046236
_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         '(C55 H88 Na2 O8 Ti), 0.5(C5 H12)'
_chemical_formula_sum            'C57.5 H94 Na2 O8 Ti'
_chemical_formula_weight         1007.22
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-14 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.135(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.5729(10)
_cell_length_b                   15.9089(4)
_cell_length_c                   17.7244(5)
_cell_measurement_reflns_used    20945
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.2000
_cell_measurement_theta_min      1.8130
_cell_volume                     11956.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_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   16.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   16.00    --  -20.00  45.00  90.00  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      0.0137325000
_diffrn_orient_matrix_UB_12      0.0225565000
_diffrn_orient_matrix_UB_13      -0.0076827000
_diffrn_orient_matrix_UB_21      -0.0027535000
_diffrn_orient_matrix_UB_22      0.0292072000
_diffrn_orient_matrix_UB_23      0.0289196000
_diffrn_orient_matrix_UB_31      0.0091399000
_diffrn_orient_matrix_UB_32      -0.0250490000
_diffrn_orient_matrix_UB_33      0.0268031000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47288
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_min         2.561
_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    0.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL O3CTi_Na2CC 2/cn2      R = 0.07
CELL   42.5729   15.9089   17.7244     90.00     95.14     90.00
SPGR C2/c
C101 0.548 0.133 0.282 !       2.82 eA-3
C102 0.485 0.158 0.262 !       2.56 eA-3
C103 0.568 0.178 0.233 !       2.09 eA-3
C104 0.500 0.141 0.254 !       1.92 eA-3
C105 0.500 0.094 0.257 !       1.87 eA-3
Q106 0.411 0.266 0.483 !       0.62 eA-3
;
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         13671
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0534P)^2^+9.2107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9589
_reflns_number_total             13671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01161c2.cif
_cod_data_source_block           o3cti_na2c10h8_n2_sq
_cod_depositor_comments
'Adding full bibliography for 7046232--7046237.cif.'
_cod_original_formula_sum        'C57.50 H94 Na2 O8 Ti'
_cod_database_code               7046236
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.966
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_platon_squeeze_void_probe_radius 1.20
_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 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.823