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_7046237
_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         'C126 H176 K4 O11 Ti2'
_chemical_formula_sum            'C126 H176 K4 O11 Ti2'
_chemical_formula_weight         2118.91
_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     direct
_audit_creation_date             2017-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-03-14 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 142.63(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.002(5)
_cell_length_b                   22.0576(10)
_cell_length_c                   39.098(8)
_cell_measurement_reflns_used    12791
_cell_measurement_temperature    123
_cell_measurement_theta_max      24.7340
_cell_measurement_theta_min      2.0470
_cell_volume                     12040(12)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -60.00 120.00   1.00   16.00    --   29.80  54.00   0.00  180
  2  \w    -60.00 120.00   1.00   16.00    --   29.80  54.00 120.00  180
  3  \w    -60.00 120.00   1.00   16.00    --   29.80  54.00 240.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_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      -0.0058013000
_diffrn_orient_matrix_UB_12      -0.0299442000
_diffrn_orient_matrix_UB_13      -0.0089774000
_diffrn_orient_matrix_UB_21      0.0167496000
_diffrn_orient_matrix_UB_22      0.0094132000
_diffrn_orient_matrix_UB_23      -0.0084564000
_diffrn_orient_matrix_UB_31      0.0476194000
_diffrn_orient_matrix_UB_32      -0.0069661000
_diffrn_orient_matrix_UB_33      0.0272175000
_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  0.1237
_diffrn_reflns_av_unetI/netI     0.1050
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            126428
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96460
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1465
_refine_ls_number_reflns         27617
_refine_ls_number_restraints     2044
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0394P)^2^+14.0427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15930
_reflns_number_total             27617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01161c2.cif
_cod_data_source_block           o3ctithf2_2kc10h8
_cod_depositor_comments
'Adding full bibliography for 7046232--7046237.cif.'
_cod_original_cell_volume        12041(8)
_cod_database_code               7046237
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.78
_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. Restrained distances
 C19-C26 \\sim C19-C526
 with sigma of 0.02
 O9-K2 \\sim O509-K2
 with sigma of 0.02
 K2-C118 \\sim K2-C618
 with sigma of 0.02
3. Rigid bond restraints
 Ti1, O1, O2, O3, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14,
 C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29,
 C526, C527, C528, C529, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39, C40,
 C41, C42, C43, C44, C45, C46, C47, C48, C49, C50, C51, C52, C53, Ti2, O4, O5,
 O6, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66, C67, C68,
 C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79, C80, C81, C82, C579,
 C580, C581, C582, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94,
 C95, C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, K1, O7,
 C107, C108, C109, C110, O8, C111, C112, C113, C114, K2, O9, C115, C116, C117,
 C118, O509, C615, C616, C617, C618, K3, O10, C119, C120, C121, C122, O11, C123,
  C124, C125, C126, K4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Ti1 \\sim O1 \\sim O2 \\sim O3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21
\\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29
\\sim C526 \\sim C527 \\sim C528 \\sim C529 \\sim C30 \\sim C31 \\sim C32 \\sim
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim Ti2 \\sim O4 \\sim O5 \\sim
O6 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C579 \\sim C580
\\sim C581 \\sim C582 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim
C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim
C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103
\\sim C104 \\sim C105 \\sim C106 \\sim K1 \\sim O7 \\sim C107 \\sim C108 \\sim
C109 \\sim C110 \\sim O8 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim K2
\\sim O9 \\sim C115 \\sim C116 \\sim C117 \\sim C118 \\sim O509 \\sim C615
\\sim C616 \\sim C617 \\sim C618 \\sim K3 \\sim O10 \\sim C119 \\sim C120 \\sim
C121 \\sim C122 \\sim O11 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim K4:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Same fragment restrains
{C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as
{C26, C27, C28, C29}
{C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as
{C526, C527, C528, C529}
{C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as
{C79, C80, C81, C82}
{C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as
{C579, C580, C581, C582}
{C122, C121, C120, C119, O10} sigma for 1-2: 0.01, 1-3: 0.01
as
{O9, C115, C116, C117, C118}
{O10, C119, C120, C121, C122} sigma for 1-2: 0.02, 1-3: 0.04
as
{O509, C615, C616, C617, C618}
6. Others
 Sof(C526)=Sof(C527)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C528)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=Sof(C529)=Sof(H52G)=Sof(H52H)=Sof(H52I)=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(C579)=Sof(C580)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C581)=Sof(H58D)=
 Sof(H58E)=Sof(H58F)=Sof(C582)=Sof(H58G)=Sof(H58H)=Sof(H58I)=1-FVAR(2)
 Sof(C79)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81)=Sof(H81A)=Sof(H81B)=
 Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(2)
 Sof(O509)=Sof(C615)=Sof(H61A)=Sof(H61B)=Sof(C616)=Sof(H61C)=Sof(H61D)=
 Sof(C617)=Sof(H61E)=Sof(H61F)=Sof(C618)=Sof(H61G)=Sof(H61H)=1-FVAR(3)
 Sof(O9)=Sof(C115)=Sof(H11N)=Sof(H11O)=Sof(C116)=Sof(H11P)=Sof(H11Q)=Sof(C117)=
 Sof(H11R)=Sof(H11S)=Sof(C118)=Sof(H11T)=Sof(H11U)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C107(H10D,H10E), C108(H10F,H10G), C109(H10H,H10I), C110(H11D,H11E), C111(H11F,
 H11G), C112(H11H,H11I), C113(H11J,H11K), C114(H11L,H11M), C115(H11N,H11O),
 C116(H11P,H11Q), C117(H11R,H11S), C118(H11T,H11U), C615(H61A,H61B), C616(H61C,
 H61D), C617(H61E,H61F), C618(H61G,H61H), C119(H11V,H11W), C120(H12A,H12B),
 C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,
 H12L), C126(H12M,H12N)
7.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C18(H18), C20(H20), C32(H32), C34(H34), C46(H46), C47(H47),
 C49(H49), C50(H50), C51(H51), C52(H52), C57(H57), C59(H59), C71(H71), C73(H73),
  C85(H85), C87(H87), C99(H99), C100(H100), C102(H102), C103(H103), C104(H104),
 C105(H105)
7.d 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), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C527(H52A,H52B,H52C), C528(H52D,H52E,H52F), C529(H52G,H52H,H52I), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C580(H58A,H58B,
 H58C), C581(H58D,H58E,H58F), C582(H58G,H58H,H58I), C90(H90A,H90B,H90C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C95(H95A,H95B,
 H95C), C96(H96A,H96B,H96C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.079
_oxdiff_exptl_absorpt_empirical_full_min 0.938