#------------------------------------------------------------------------------
#$Date: 2018-08-29 02:59:35 +0300 (Wed, 29 Aug 2018) $
#$Revision: 210209 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/10/4301057.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4301057
loop_
_publ_author_name
'Adams, Nico'
'Bigmore, Helen R.'
'Blundell, Timothy L.'
'Boyd, Catherine L.'
'Dubberley, Stuart R.'
'Sealey, Andrew J.'
'Cowley, Andrew R.'
'Skinner, Michael E. G.'
'Mountford, Philip'
_publ_section_title
;
 New Titanium Imido Synthons: Syntheses and Supramolecular Structures
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2882
_journal_page_last               2894
_journal_paper_doi               10.1021/ic050011z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         ' C10 H14 Cl2 F5 N3 Ti1 '
_chemical_formula_sum            'C10 H14 Cl2 F5 N3 Ti'
_chemical_formula_weight         390.04
_chemical_melting_point          ?
_chemical_name_systematic        Ti(NC6F5)Cl2(NHMe2)2
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 109.69(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.696(3)
_cell_length_b                   15.569(1)
_cell_length_c                   6.7371(9)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    200
_cell_measurement_theta_max      32
_cell_measurement_theta_min      22
_cell_volume                     1550.1(4)
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.08
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3439
_diffrn_reflns_theta_max         74.27
_diffrn_reflns_theta_min         4.12
_diffrn_standards_decay_%        32.61
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.334
_exptl_absorpt_correction_T_max  0.04
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 

 Azimutal absorption correction (North et al, 1968) 

;
_exptl_crystal_colour            'orange '
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'fragment '
_exptl_crystal_F_000             789.960
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.60
_refine_ls_extinction_coef       67.5(57)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0778
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1536
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.002145
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 

 14.1    -1.25     9.02    

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0648
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1536
_reflns_number_total             1581
_reflns_threshold_expression     >3.00σ(I)
_cod_data_source_file            ic050011zsi20050104_034133_4.cif
_cod_data_source_block           COMPOUND_9
_cod_depositor_comments
;

The following automatic conversions were performed:

_chemical_melting_point value 'not measured' changed to '?' - value

is undefined or not given.



Automatic conversion script

Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 


The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1550.1(3)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C10 H14 Cl2 F5 N3 Ti1 '
_cod_database_code               4301057
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Ti1 0.0000 -0.20170(4) 0.7500 0.0251 1.0000 Uani
Cl1 0.09906(5) -0.15376(5) 1.07447(11) 0.0363 1.0000 Uani
F1 -0.15240(12) -0.40633(13) 0.5278(3) 0.0450 1.0000 Uani
F2 -0.15230(16) -0.57823(14) 0.5305(4) 0.0550 1.0000 Uani
F3 0.0000 -0.66544(17) 0.7500 0.0609 1.0000 Uani
N1 0.0000 -0.3112(2) 0.7500 0.0298 1.0000 Uani
N2 -0.10605(15) -0.17331(15) 0.8866(4) 0.0281 1.0000 Uani
C1 0.0000 -0.3985(2) 0.7500 0.0247 1.0000 Uani
C2 -0.07672(19) -0.44724(19) 0.6398(4) 0.0298 1.0000 Uani
C3 -0.0770(2) -0.5353(2) 0.6405(5) 0.0355 1.0000 Uani
C4 0.0000 -0.5796(3) 0.7500 0.0389 1.0000 Uani
C5 -0.1248(2) -0.0802(2) 0.8901(6) 0.0432 1.0000 Uani
C6 -0.1924(2) -0.2207(2) 0.7936(5) 0.0370 1.0000 Uani
H21 -0.0822 -0.1922 1.0150 0.0373 1.0000 Uiso
H51 -0.0666 -0.0483 0.9529 0.0590 1.0000 Uiso
H52 -0.1645 -0.0698 0.9770 0.0590 1.0000 Uiso
H53 -0.1562 -0.0595 0.7430 0.0590 1.0000 Uiso
H61 -0.1796 -0.2835 0.7913 0.0494 1.0000 Uiso
H62 -0.2320 -0.2104 0.8804 0.0494 1.0000 Uiso
H63 -0.2237 -0.2000 0.6464 0.0494 1.0000 Uiso
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0254(4) 0.0167(4) 0.0350(4) 0.0000 0.0124(3) 0.0000
Cl1 0.0333(4) 0.0369(4) 0.0383(4) -0.0062(3) 0.0116(3) -0.0026(3)
F1 0.0300(9) 0.0466(11) 0.0517(11) -0.0016(9) 0.0047(8) 0.0016(8)
F2 0.0592(13) 0.0474(12) 0.0644(13) -0.020(1) 0.0288(11) -0.033(1)
F3 0.106(3) 0.0160(12) 0.078(2) 0.0000 0.054(2) 0.0000
N1 0.0296(17) 0.0230(16) 0.0384(18) 0.0000 0.0135(14) 0.0000
N2 0.0262(11) 0.0230(11) 0.0368(12) 0.0041(9) 0.0128(9) 0.0020(9)
C1 0.0272(17) 0.0201(17) 0.0292(17) 0.0000 0.0125(14) 0.0000
C2 0.0287(14) 0.0285(14) 0.0345(14) -0.0012(11) 0.0136(11) -0.002(1)
C3 0.0444(17) 0.0287(15) 0.0406(16) -0.0070(12) 0.0237(14) -0.0133(13)
C4 0.066(3) 0.0182(18) 0.046(2) 0.0000 0.036(2) 0.0000
C5 0.0460(18) 0.0242(15) 0.066(2) -0.0071(14) 0.0277(16) 0.0041(13)
C6 0.0289(14) 0.0321(15) 0.0530(18) 0.0026(14) 0.0178(13) -0.0021(12)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C   ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl  ' 0.3480 0.7020 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'F   ' 0.0690 0.0530 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'Ti  ' 0.1890 1.8070 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Ti1 . Cl1 5_556 142.75(5) yes
Cl1 . Ti1 . N1 . 108.62(2) yes
Cl1 5_556 Ti1 . N1 . 108.62(2) yes
Cl1 . Ti1 . N2 . 84.45(7) yes
Cl1 5_556 Ti1 . N2 . 88.19(6) yes
N1 . Ti1 . N2 . 101.58(6) yes
Cl1 . Ti1 . N2 5_556 88.19(6) yes
Cl1 5_556 Ti1 . N2 5_556 84.45(7) yes
N1 . Ti1 . N2 5_556 101.58(6) yes
N2 . Ti1 . N2 5_556 156.83(13) yes
Ti1 . N1 . C1 . 180 yes
Ti1 . N2 . C5 . 112.70(19) yes
Ti1 . N2 . C6 . 115.81(19) yes
C5 . N2 . C6 . 109.6(2) yes
N1 . C1 . C2 . 122.67(17) yes
N1 . C1 . C2 5_556 122.67(17) yes
C2 . C1 . C2 5_556 114.7(3) yes
F1 . C2 . C1 . 118.8(3) yes
F1 . C2 . C3 . 118.4(3) yes
C1 . C2 . C3 . 122.7(3) yes
F2 . C3 . C2 . 119.9(3) yes
F2 . C3 . C4 . 119.9(3) yes
C2 . C3 . C4 . 120.2(3) yes
F3 . C4 . C3 . 120.24(19) yes
F3 . C4 . C3 5_556 120.24(19) yes
C3 . C4 . C3 5_556 119.5(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . Cl1 . 2.3373(7) yes
Ti1 . Cl1 5_556 2.3373(7) yes
Ti1 . N1 . 1.706(3) yes
Ti1 . N2 . 2.201(2) yes
Ti1 . N2 5_556 2.201(2) yes
F1 . C2 . 1.335(3) yes
F2 . C3 . 1.343(4) yes
F3 . C4 . 1.336(5) yes
N1 . C1 . 1.359(5) yes
N2 . C5 . 1.482(4) yes
N2 . C6 . 1.483(4) yes
N2 . H21 . 0.870 no
C1 . C2 . 1.405(3) yes
C1 . C2 5_556 1.405(3) yes
C2 . C3 . 1.370(4) yes
C3 . C4 . 1.371(4) yes
