#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/47/7034799.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_7034799
loop_
_publ_author_name
'Bhalla, Rajiv'
'Levason, William'
'Luthra, Sajinder K.'
'McRobbie, Graeme'
'Monzittu, Francesco M.'
'Palmer, Jazmyn'
'Reid, Gillian'
'Sanderson, George'
'Zhang, Wenjian'
_publ_section_title
;
 Hydrothermal synthesis of Group 13 metal trifluoride complexes with
 neutral N-donor ligands.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9569
_journal_page_last               9580
_journal_paper_doi               10.1039/c5dt01120e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'Cl, C7 H17 N2'
_chemical_formula_sum            'C7 H17 Cl N2'
_chemical_formula_weight         164.8
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3293(6)
_cell_length_b                   10.3564(7)
_cell_length_c                   10.3564(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     893.36(11)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.010329
_diffrn_orient_matrix_UB_12      0.049982
_diffrn_orient_matrix_UB_13      0.108669
_diffrn_orient_matrix_UB_21      0.020657
_diffrn_orient_matrix_UB_22      -0.086423
_diffrn_orient_matrix_UB_23      0.037787
_diffrn_orient_matrix_UB_31      0.093957
_diffrn_orient_matrix_UB_32      0.015447
_diffrn_orient_matrix_UB_33      -0.016035
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8132
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0354
_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/[σ²(Fo²)+(0.0385P)²+0.4058P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.689
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                1799
_reflns_number_total             2024
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01120e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7034798--7034806.cif.'
_cod_original_formula_sum        'C7 H17 Cl1 N2 '
_cod_database_code               7034799
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2014-1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_file
;
TITL shelx in P2(1)2(1)2(1)
CELL 0.71073 8.3293 10.3564 10.3564 90 90 90
ZERR 4 0.0006 0.0007 0.0007 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z

SFAC C H Cl N
UNIT 28 68 4 8

L.S. 50
PLAN  5
TEMP 100.15
BOND
MORE -1
CONF
fmap 2
acta
REM <HKL>//soton.ac.uk/ude/personalfiles/users/fmm1u13/mydesktop/Structures/FM
REM M9-B.Bob/shelx.hkl</HKL>

WGHT    0.038500    0.405800
FVAR       0.51456
CL1   3    0.224289    0.768087    0.281882    11.00000    0.01591    0.01772 =
         0.02063    0.00106    0.00107    0.00103
N1    4    0.178192    0.858005    0.663162    11.00000    0.01092    0.01255 =
         0.01338    0.00160    0.00158    0.00044
N2    4    0.223760    0.667128    0.865432    11.00000    0.01383    0.01194 =
         0.01260    0.00094   -0.00068   -0.00049
C1    1    0.164885    0.713914    0.640251    11.00000    0.01577    0.01167 =
         0.01520   -0.00016   -0.00065   -0.00255
AFIX  23
H1A   2    0.053917    0.687545    0.650833    11.00000   -1.20000
H1B   2    0.196550    0.694710    0.552187    11.00000   -1.20000
AFIX   0
C2    1    0.269511    0.637451    0.732551    11.00000    0.01631    0.01136 =
         0.01705   -0.00033    0.00095    0.00119
AFIX  23
H2A   2    0.256411    0.545782    0.716481    11.00000   -1.20000
H2B   2    0.381446    0.659426    0.718948    11.00000   -1.20000
AFIX   0
C3    1    0.247049    0.805066    0.891524    11.00000    0.01615    0.01631 =
         0.01438   -0.00232   -0.00017   -0.00124
AFIX  23
H3A   2    0.358830    0.827650    0.878103    11.00000   -1.20000
H3B   2    0.220155    0.823368    0.980798    11.00000   -1.20000
AFIX   0
C4    1    0.142303    0.885135    0.803371    11.00000    0.01675    0.01253 =
         0.01381   -0.00063    0.00525    0.00280
AFIX  23
H4A   2    0.030352    0.866083    0.820766    11.00000   -1.20000
H4B   2    0.160017    0.976021    0.820962    11.00000   -1.20000
AFIX   0
C5    1    0.340445    0.907559    0.625914    11.00000    0.01378    0.01672 =
         0.01875    0.00145    0.00393   -0.00164
AFIX 137
H5A   2    0.355616    0.896904    0.534644    11.00000   -1.50000
H5B   2    0.421579    0.860114    0.671558    11.00000   -1.50000
H5C   2    0.348244    0.997455    0.647639    11.00000   -1.50000
AFIX   0
C6    1    0.054199    0.925730    0.582002    11.00000    0.01568    0.01918 =
         0.02138    0.00574   -0.00120    0.00369
AFIX 137
H6A   2    0.076455    0.910860    0.492274    11.00000   -1.50000
H6B   2    0.057494    1.016746    0.599369    11.00000   -1.50000
H6C   2   -0.050445    0.892782    0.602594    11.00000   -1.50000
AFIX   0
C7    1    0.318950    0.590841    0.956132    11.00000    0.02177    0.01986 =
         0.01817    0.00339   -0.00331    0.00130
AFIX 137
H7A   2    0.306080    0.500707    0.937123    11.00000   -1.50000
H7B   2    0.283196    0.607679    1.042631    11.00000   -1.50000
H7C   2    0.430111    0.614019    0.948229    11.00000   -1.50000
AFIX   0
HKLF 4

REM  shelx in P2(1)2(1)2(1)
REM R1 =  0.0354 for    1799 Fo > 4sig(Fo)  and  0.0448 for all    2024 data
REM     94 parameters refined using      0 restraints

END

WGHT      0.0279      0.2968

REM Highest difference peak  0.234,  deepest hole -0.230,  1-sigma level  0.050
Q1    1   0.2734  0.6791  0.2783  11.00000  0.05    0.23
Q2    1   0.2366  0.7375  0.8759  11.00000  0.05    0.20
Q3    1   0.2133  0.7642  0.1941  11.00000  0.05    0.19
Q4    1   0.1610  0.7979  0.3777  11.00000  0.05    0.18
Q5    1   0.2347  0.6514  0.8147  11.00000  0.05    0.18
;
_shelx_res_checksum              23220
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Cl1 Cl 0.22429(8) 0.76809(6) 0.28188(6) 0.01808(17) Uani 1 1 d .
N1 N 0.1782(3) 0.8580(2) 0.6632(2) 0.0123(5) Uani 1 1 d .
N2 N 0.2238(3) 0.6671(2) 0.8654(2) 0.0128(5) Uani 1 1 d .
C1 C 0.1649(3) 0.7139(3) 0.6403(3) 0.0142(6) Uani 1 1 d .
H1A H 0.0539 0.6875 0.6508 0.017 Uiso 1 1 calc R
H1B H 0.1965 0.6947 0.5522 0.017 Uiso 1 1 calc R
C2 C 0.2695(3) 0.6375(2) 0.7326(2) 0.0149(5) Uani 1 1 d .
H2A H 0.2564 0.5458 0.7165 0.018 Uiso 1 1 calc R
H2B H 0.3814 0.6594 0.7189 0.018 Uiso 1 1 calc R
C3 C 0.2470(3) 0.8051(2) 0.8915(2) 0.0156(6) Uani 1 1 d .
H3A H 0.3588 0.8277 0.8781 0.019 Uiso 1 1 calc R
H3B H 0.2202 0.8234 0.9808 0.019 Uiso 1 1 calc R
C4 C 0.1423(3) 0.8851(3) 0.8034(3) 0.0144(6) Uani 1 1 d .
H4A H 0.0304 0.8661 0.8208 0.017 Uiso 1 1 calc R
H4B H 0.1600 0.9760 0.8210 0.017 Uiso 1 1 calc R
C5 C 0.3404(3) 0.9076(3) 0.6259(3) 0.0164(6) Uani 1 1 d .
H5A H 0.3556 0.8969 0.5346 0.025 Uiso 1 1 calc GR
H5B H 0.4216 0.8601 0.6716 0.025 Uiso 1 1 calc GR
H5C H 0.3482 0.9975 0.6476 0.025 Uiso 1 1 calc GR
C6 C 0.0542(4) 0.9257(3) 0.5820(3) 0.0187(6) Uani 1 1 d .
H6A H 0.0765 0.9109 0.4923 0.028 Uiso 1 1 calc GR
H6B H 0.0575 1.0167 0.5994 0.028 Uiso 1 1 calc GR
H6C H -0.0504 0.8928 0.6026 0.028 Uiso 1 1 calc GR
C7 C 0.3189(4) 0.5908(3) 0.9561(3) 0.0199(6) Uani 1 1 d .
H7A H 0.3061 0.5007 0.9371 0.030 Uiso 1 1 calc GR
H7B H 0.2832 0.6077 1.0426 0.030 Uiso 1 1 calc GR
H7C H 0.4301 0.6140 0.9482 0.030 Uiso 1 1 calc GR
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
Cl1 0.0159(3) 0.0177(3) 0.0206(3) 0.0011(3) 0.0011(2) 0.0010(2)
N1 0.0109(11) 0.0126(11) 0.0134(11) 0.0016(9) 0.0016(8) 0.0004(9)
N2 0.0138(11) 0.0119(10) 0.0126(10) 0.0009(8) -0.0007(9) -0.0005(10)
C1 0.0158(12) 0.0117(13) 0.0152(13) -0.0002(11) -0.0006(10) -0.0026(11)
C2 0.0163(13) 0.0114(11) 0.0170(13) -0.0003(10) 0.0009(11) 0.0012(11)
C3 0.0161(15) 0.0163(13) 0.0144(13) -0.0023(10) -0.0002(11) -0.0012(11)
C4 0.0167(13) 0.0125(13) 0.0138(13) -0.0006(10) 0.0052(11) 0.0028(10)
C5 0.0138(13) 0.0167(14) 0.0188(14) 0.0015(12) 0.0039(11) -0.0016(11)
C6 0.0157(14) 0.0192(15) 0.0214(14) 0.0057(12) -0.0012(11) 0.0037(12)
C7 0.0218(16) 0.0199(14) 0.0182(14) 0.0034(12) -0.0033(11) 0.0013(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C4 N1 C1 108.6(2)
C5 N1 C1 111.3(2)
C5 N1 C4 111.3(2)
C5 N1 C6 108.4(2)
C6 N1 C1 108.7(2)
C6 N1 C4 108.3(2)
C2 N2 C3 110.1(2)
C7 N2 C2 110.5(2)
C7 N2 C3 109.7(2)
C2 C1 N1 111.9(2)
N2 C2 C1 109.5(2)
N2 C3 C4 110.3(2)
N1 C4 C3 111.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.515(3)
N1 C4 1.509(3)
N1 C5 1.496(3)
N1 C6 1.505(4)
N2 C2 1.461(3)
N2 C3 1.467(3)
N2 C7 1.461(3)
C1 C2 1.517(4)
C3 C4 1.511(4)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 C1 C2 N2 58.2(3)
N2 C3 C4 N1 -58.3(3)
C1 N1 C4 C3 53.9(3)
C2 N2 C3 C4 61.3(3)
C3 N2 C2 C1 -60.8(3)
C4 N1 C1 C2 -54.1(3)
C5 N1 C1 C2 68.7(3)
C5 N1 C4 C3 -69.1(3)
C6 N1 C1 C2 -171.9(2)
C6 N1 C4 C3 171.8(2)
C7 N2 C2 C1 177.9(2)
C7 N2 C3 C4 -176.9(2)
