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_7046235
_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         'C73 H102 K2 O7 Ti, C4 H8 O'
_chemical_formula_sum            'C77 H110 K2 O8 Ti'
_chemical_formula_weight         1289.74
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-03-14 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 138.195(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6112(9)
_cell_length_b                   35.8757(6)
_cell_length_c                   22.0952(15)
_cell_measurement_reflns_used    31156
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.7210
_cell_measurement_theta_min      2.8660
_cell_volume                     7192(2)
_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 0.993
_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   -120.00  60.00   0.50    4.00    --  -30.00  45.00   0.00  360
  2  \w   -120.00  60.00   0.50    4.00    --  -30.00  45.00  90.00  360
  3  \w   -120.00  60.00   0.50    4.00    --  -30.00  45.00 180.00  360
  4  \w   -120.00  60.00   0.50    4.00    --  -30.00  45.00 270.00  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      0.0777901000
_diffrn_orient_matrix_UB_12      -0.0019501000
_diffrn_orient_matrix_UB_13      0.0358601000
_diffrn_orient_matrix_UB_21      -0.0076524000
_diffrn_orient_matrix_UB_22      -0.0193606000
_diffrn_orient_matrix_UB_23      0.0021874000
_diffrn_orient_matrix_UB_31      -0.0010471000
_diffrn_orient_matrix_UB_32      -0.0034969000
_diffrn_orient_matrix_UB_33      -0.0320746000
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81103
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         3.102
_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    0.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90400
_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 violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         16460
_refine_ls_number_restraints     924
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0590P)^2^+6.0430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11472
_reflns_number_total             16460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01161c2.cif
_cod_data_source_block           o3ctianth_2nd
_cod_depositor_comments
'Adding full bibliography for 7046232--7046237.cif.'
_cod_original_cell_volume        7192.1(14)
_cod_database_code               7046235
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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. Rigid bond restraints
 C26, C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C62, C63, C64, C65, O105, C162, C163, C164, C165
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C66, C67, C68, C69, O106, C166, C167, C168, C169, O7, C70, C71, C72, C73,
 O107, C170, C171, C172, C173, O8, C74, C75, C76, C77, C174, C175, C176, C177
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
O5 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim O105 \\sim C162 \\sim C163
\\sim C164 \\sim C165: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
O6 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim O106 \\sim C166 \\sim C167
\\sim C168 \\sim C169 \\sim O7 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim
O107 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim O8 \\sim C74 \\sim C75
\\sim C76 \\sim C77 \\sim C174 \\sim C175 \\sim C176 \\sim C177: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Same fragment restrains
{C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.04
as
{C26, C27, C28, C29}
{C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.04
as
{C126, C127, C128, C129}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5, C62, C63, C64, C65}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{O105, C162, C163, C164, C165}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6, C66, C67, C68, C69}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{O106, C166, C167, C168, C169}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7, C70, C71, C72, C73}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.02, 1-3: 0.04
as
{O107, C170, C171, C172, C173}
{O4, C58, C59, C60, C61} sigma for 1-2: 0.01, 1-3: 0.01
as
{O8, C74, C75, C76, C77}
{C74, C75, C76, C77} sigma for 1-2: 0.01, 1-3: 0.01
as
{C174, C175, C176, C177}
5. Others
 Sof(C126)=Sof(C127)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C128)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C129)=Sof(H12G)=Sof(H12H)=Sof(H12I)=1-FVAR(1)
 Sof(C26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(O105)=Sof(C162)=Sof(H16A)=Sof(H16B)=Sof(C163)=Sof(H16C)=Sof(H16D)=
 Sof(C164)=Sof(H16E)=Sof(H16F)=Sof(C165)=Sof(H16G)=Sof(H16H)=1-FVAR(2)
 Sof(O5)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=
 Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=FVAR(2)
 Sof(O106)=Sof(C166)=Sof(H16I)=Sof(H16J)=Sof(C167)=Sof(H16K)=Sof(H16L)=
 Sof(C168)=Sof(H16M)=Sof(H16N)=Sof(C169)=Sof(H16O)=Sof(H16P)=1-FVAR(3)
 Sof(O6)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=
 Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(3)
 Sof(O107)=Sof(C170)=Sof(H17A)=Sof(H17B)=Sof(C171)=Sof(H17C)=Sof(H17D)=
 Sof(C172)=Sof(H17E)=Sof(H17F)=Sof(C173)=Sof(H17G)=Sof(H17H)=1-FVAR(4)
 Sof(O7)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=
 Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=Sof(H73B)=FVAR(4)
 Sof(C174)=Sof(H17I)=Sof(H17J)=Sof(C175)=Sof(H17K)=Sof(H17L)=Sof(C176)=
 Sof(H17M)=Sof(H17N)=Sof(C177)=Sof(H17O)=Sof(H17P)=1-FVAR(5)
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=
 Sof(H76B)=Sof(C77)=Sof(H77A)=Sof(H77B)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,
 H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C162(H16A,H16B),
 C163(H16C,H16D), C164(H16E,H16F), C165(H16G,H16H), C66(H66A,H66B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C166(H16I,H16J), C167(H16K,H16L),
 C168(H16M,H16N), C169(H16O,H16P), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,
 H72B), C73(H73A,H73B), C170(H17A,H17B), C171(H17C,H17D), C172(H17E,H17F),
 C173(H17G,H17H), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C174(H17I,H17J), C175(H17K,H17L), C176(H17M,H17N), C177(H17O,H17P)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C18(H18), C20(H20), C32(H32), C34(H34), C50(H50), C51(H51),
 C53(H53), C54(H54), C55(H55), C56(H56)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C127(H12A,H12B,H12C), C128(H12D,H12E,H12F), C129(H12G,
 H12H,H12I), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.863