An air-stable organometallic polymer containing titanafluorene moieties obtained by the Sonogashira-Hagihara cross-coupling polycondensation.
Tanudjaja, Alvin; Inagi, Shinsuke; Kitamura, Fusao; Takata, Toshikazu; Tomita, Ikuyoshi; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3037–3043; doi:10.1039/d0dt03663c

data_7706532
_publ_section_title
;
 An air-stable organometallic polymer containing titanafluorene moieties
 obtained by the Sonogashira-Hagihara cross-coupling polycondensation.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3037
_journal_page_last               3043
_journal_paper_doi               10.1039/d0dt03663c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C22 H16 Br2 Ti, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.5 H17 Br2 Cl Ti'
_chemical_formula_weight         530.53
_chemical_melting_point          458.0(10)
_chemical_name_common
2,7?-dibromo-9-bis(cyclopentadienyl)titanafluorene
_chemical_name_systematic
2,7?-dibromo-9-bis(cyclopentadienyl)titanafluorene
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-04 deposited with the CCDC.	2021-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.445(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2921(2)
_cell_length_b                   14.6419(4)
_cell_length_c                   14.6728(3)
_cell_measurement_reflns_used    18187
_cell_measurement_temperature    90
_cell_measurement_theta_max      74.5430
_cell_measurement_theta_min      4.2450
_cell_volume                     1969.23(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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    124.00 150.00   0.50    0.06    --  106.13  80.00  84.00   52
  2  \w     84.00 178.00   0.50    0.06    --  106.13  45.00  60.00  188
  3  \w     40.00  65.00   0.50    0.05    --   42.05  80.00  84.00   50
  4  \w     83.00 176.00   0.50    0.06    --  106.13  30.00  30.00  186
  5  \w    134.00 178.00   0.50    0.06    --  106.13  61.00-180.00   88
  6  \w     34.00 105.00   0.50    0.06    --  106.13 -94.00 -30.00  142
  7  \w     57.00  94.00   0.50    0.05    --   42.05-125.00-150.00   74
  8  \w     20.00  52.00   0.50    0.05    --   42.05-125.00-150.00   64
  9  \w     18.00  96.00   0.50    0.05    --   42.05-125.00 -30.00  156
 10  \w     47.00  97.00   0.50    0.06    --  106.13 -94.00  60.00  100
 11  \w     34.00  68.00   0.50    0.06    --  106.13 -61.00  60.00   68
 12  \w     44.00  69.00   0.50    0.06    --  106.13 -61.00 120.00   50
 13  \w     -4.00  21.00   0.50    0.05    --   42.05 -80.00 -39.00   50
 14  \w     35.00 103.00   0.50    0.06    --  106.13 -77.00-180.00  136
 15  \w     60.00  85.00   0.50    0.06    --  106.13 -80.00 -39.00   50
 16  \w     32.00  72.00   0.50    0.06    --  106.13 -61.00 -30.00   80
 17  \w    -70.00 -28.00   0.50    0.05    --  -42.05  80.00  84.00   84
 18  \w    -24.00   8.00   0.50    0.05    --  -42.05  80.00  84.00   64
 19  \w     -9.00  39.00   0.50    0.05    --  -42.05  19.00  90.00   96
 20  \w    -24.00  33.00   0.50    0.05    --  -42.05  19.00  60.00  114
 21  \w     -1.00  38.00   0.50    0.05    --  -42.05  19.00 -60.00   78
 22  \w    -39.00  29.00   0.50    0.05    --  -42.05  37.00-180.00  136
 23  \w    -67.00 -29.00   0.50    0.06    -- -102.00  61.00 -60.00   76
 24  \w    -59.00 -34.00   0.50    0.06    -- -102.00  61.00 -90.00   50
 25  \w    -69.00 -29.00   0.50    0.06    -- -102.00  61.00   0.00   80
 26  \w    -67.00 -32.00   0.50    0.06    -- -102.00  61.00  60.00   70
 27  \w    -65.00 -30.00   0.50    0.06    -- -102.00  61.00  90.00   70
 28  \w    -55.00 -28.00   0.50    0.06    -- -102.00  61.00 150.00   54
 29  \w    -73.00 -44.00   0.50    0.06    -- -102.00  80.00  84.00   58
 30  \w   -125.00 -89.00   0.50    0.06    -- -102.00  80.00  84.00   72
 31  \w    -61.00 -36.00   0.50    0.06    -- -102.00  61.00-150.00   50
 32  \w   -116.00 -13.00   0.50    0.05    --  -42.05 -80.00 -39.00  206
 33  \w   -105.00 -76.00   0.50    0.06    -- -102.00 -77.00 -60.00   58
 34  \w   -164.00-111.00   0.50    0.06    -- -102.00 -77.00 -60.00  106
 35  \w   -148.00-123.00   0.50    0.06    -- -102.00 -80.00 -39.00   50
 36  \w   -148.00-122.00   0.50    0.06    -- -102.00 -45.00   0.00   52
 37  \w   -114.00 -89.00   0.50    0.06    -- -102.00 -45.00   0.00   50
 38  \w   -118.00 -81.00   0.50    0.06    -- -102.00 -45.00 -60.00   74
 39  \w   -174.00 -84.00   0.50    0.06    -- -102.00 -30.00-180.00  180
 40  \w   -175.00 -88.00   0.50    0.06    -- -102.00 -30.00-150.00  174
 41  \w   -145.00 -78.00   0.50    0.06    -- -102.00 -30.00-120.00  134
 42  \w   -168.00-143.00   0.50    0.06    -- -102.00 -45.00 -60.00   50
 43  \w   -145.00-119.00   0.50    0.06    -- -102.00 -30.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23426
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.687
_diffrn_reflns_theta_min         4.295
_exptl_absorpt_coefficient_mu    9.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / hexane'
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 3461 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7706
_refine_ls_number_restraints     631
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+1.8368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                7595
_reflns_number_total             7706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03663c2.cif
_cod_data_source_block           dibromotitan
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '457-459' was changed to
'458.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7706532.cif.

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C45 H34 Br4 Cl2 Ti2'
_cod_original_formula_weight         1061.06
_cod_original_formula_moiety         '2(C22 H16 Br2 Ti), C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_database_code               7706532
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.550
_shelx_estimated_absorpt_t_min   0.154
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C57(H57), C35(H35), C40(H40), C41(H41), C37(H37), C53(H53), C42(H42),
 C17(H17), C34(H34), C38(H38), C18(H18), C52(H52), C14(H14), C43(H43), C36(H36),
  C13(H13), C12(H12), C11(H11), C10(H10), C58(H58)
3.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B)
3.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C55(H55), C44(H44), C28(H28), C6(H6), C54(H54), C47(H47), C22(H22),
 C19(H19), C27(H27), C20(H20), C45(H45)
;
_shelx_res_checksum              92460
_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
;