#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:05:52 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230042 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/56/7045688.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_7045688
loop_
_publ_author_name
'Wang, Peng'
'Chao, Jianbin'
'Chen, Xia'
_publ_section_title
;
 Living ring-opening polymerization of ε-caprolactone catalyzed by
 β-quinolyl-enamino aluminium complexes: ligand electronic effects.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4118
_journal_page_last               4127
_journal_paper_doi               10.1039/c7dt04522k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C24 H17 F3 N2'
_chemical_formula_weight         390.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1627(5)
_cell_length_b                   7.2645(3)
_cell_length_c                   20.2474(7)
_cell_measurement_reflns_used    8625
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.302
_cell_measurement_theta_min      2.994
_cell_volume                     1854.88(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17402
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         2.994
_exptl_absorpt_coefficient_mu    0.104
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0466
_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/[σ²(Fo²)+(0.0637P)²+0.7125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3667
_reflns_number_total             4596
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04522k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045687--7045691.cif.'
_cod_database_code               7045688
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_refinement_flags_adp
N2 N 0.70199(9) 0.84584(18) 0.15878(5) 0.0312(3) Uani 1 1 d . .
H2 H 0.6581 0.8819 0.1818 0.037 Uiso 1 1 calc R U
N1 N 0.50841(9) 0.71076(16) 0.14736(6) 0.0291(3) Uani 1 1 d . .
C1 C 0.49161(11) 0.71682(19) 0.07932(7) 0.0287(3) Uani 1 1 d . .
C22 C 0.99342(11) 0.6380(2) 0.27920(7) 0.0343(3) Uani 1 1 d . .
C4 C 0.34267(11) 0.5419(2) 0.13081(8) 0.0336(3) Uani 1 1 d . .
C12 C 0.73967(11) 0.95652(19) 0.05338(7) 0.0287(3) Uani 1 1 d . .
C20 C 0.86867(11) 0.6829(2) 0.16691(7) 0.0302(3) Uani 1 1 d . .
H20 H 0.8497 0.6644 0.1185 0.036 Uiso 1 1 calc R U
C19 C 0.80084(11) 0.77717(19) 0.19680(6) 0.0274(3) Uani 1 1 d . .
C21 C 0.96357(11) 0.6169(2) 0.20862(8) 0.0328(3) Uani 1 1 d . .
C9 C 0.43558(11) 0.62517(19) 0.17348(7) 0.0298(3) Uani 1 1 d . .
C23 C 0.92474(12) 0.7295(2) 0.30780(7) 0.0344(3) Uani 1 1 d . .
C11 C 0.66790(11) 0.86129(19) 0.08701(6) 0.0280(3) Uani 1 1 d . .
C8 C 0.45523(12) 0.6203(2) 0.24568(8) 0.0360(3) Uani 1 1 d . .
H8 H 0.5172 0.6767 0.2746 0.043 Uiso 1 1 calc R U
C10 C 0.56889(11) 0.8072(2) 0.05118(7) 0.0295(3) Uani 1 1 d . .
H10 H 0.5478 0.8304 0.0030 0.035 Uiso 1 1 calc R U
C24 C 0.83000(11) 0.8008(2) 0.26844(7) 0.0316(3) Uani 1 1 d . .
H24 H 0.7848 0.8654 0.2896 0.038 Uiso 1 1 calc R U
C3 C 0.32652(12) 0.5522(2) 0.05850(8) 0.0365(3) Uani 1 1 d . .
H3 H 0.2650 0.4991 0.0278 0.044 Uiso 1 1 calc R U
C7 C 0.38522(14) 0.5345(2) 0.27425(9) 0.0437(4) Uani 1 1 d . .
H7 H 0.3992 0.5313 0.3230 0.052 Uiso 1 1 calc R U
C13 C 0.73330(12) 0.9264(2) -0.01596(7) 0.0318(3) Uani 1 1 d . .
H13 H 0.6834 0.8403 -0.0421 0.038 Uiso 1 1 calc R U
C2 C 0.39909(11) 0.6379(2) 0.03316(7) 0.0340(3) Uani 1 1 d . .
H2A H 0.3882 0.6453 -0.0152 0.041 Uiso 1 1 calc R U
C16 C 0.87923(12) 1.1776(2) 0.05851(8) 0.0366(3) Uani 1 1 d . .
H16 H 0.9292 1.2637 0.0845 0.044 Uiso 1 1 calc R U
C17 C 0.81329(12) 1.0852(2) 0.08975(7) 0.0336(3) Uani 1 1 d . .
H17 H 0.8183 1.1098 0.1367 0.040 Uiso 1 1 calc R U
C14 C 0.79895(12) 1.0207(2) -0.04684(7) 0.0354(3) Uani 1 1 d . .
H14 H 0.7928 0.9989 -0.0941 0.043 Uiso 1 1 calc R U
C18 C 0.94532(15) 1.2472(2) -0.04442(10) 0.0471(4) Uani 1 1 d . .
H18A H 0.9777 1.3527 -0.0160 0.071 Uiso 1 1 calc R U
H18B H 0.9037 1.2906 -0.0900 0.071 Uiso 1 1 calc R U
H18C H 1.0011 1.1637 -0.0495 0.071 Uiso 1 1 calc R U
C6 C 0.29298(14) 0.4511(2) 0.23227(10) 0.0470(4) Uani 1 1 d . .
H6 H 0.2450 0.3920 0.2526 0.056 Uiso 1 1 calc R U
C5 C 0.27208(13) 0.4549(2) 0.16214(10) 0.0430(4) Uani 1 1 d . .
H5 H 0.2094 0.3983 0.1341 0.052 Uiso 1 1 calc R U
C15 C 0.87376(12) 1.1467(2) -0.01026(8) 0.0347(3) Uani 1 1 d . .
F1 F 1.02991(8) 0.52600(15) 0.17990(5) 0.0476(3) Uani 1 1 d . .
F2 F 1.08700(7) 0.57384(14) 0.31848(5) 0.0492(3) Uani 1 1 d . .
F3 F 0.95362(9) 0.75179(15) 0.37678(4) 0.0516(3) Uani 1 1 d . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C11 N2 C19 124.85(11)
C1 N1 C9 119.16(12)
N1 C1 C2 121.48(13)
N1 C1 C10 119.47(12)
C2 C1 C10 119.05(12)
F2 C22 C23 121.32(13)
F2 C22 C21 121.04(15)
C23 C22 C21 117.64(13)
C5 C4 C9 118.74(15)
C5 C4 C3 124.20(15)
C9 C4 C3 117.07(13)
C17 C12 C13 117.86(13)
C17 C12 C11 120.48(12)
C13 C12 C11 121.61(12)
C21 C20 C19 119.07(12)
C20 C19 C24 119.37(13)
C20 C19 N2 123.12(12)
C24 C19 N2 117.48(12)
F1 C21 C22 118.25(13)
F1 C21 C20 119.35(13)
C22 C21 C20 122.39(14)
N1 C9 C8 118.09(13)
N1 C9 C4 122.43(13)
C8 C9 C4 119.48(14)
F3 C23 C24 119.67(15)
F3 C23 C22 118.02(13)
C24 C23 C22 122.29(13)
C10 C11 N2 120.43(13)
C10 C11 C12 122.02(12)
N2 C11 C12 117.24(12)
C7 C8 C9 120.21(15)
C11 C10 C1 126.39(12)
C23 C24 C19 119.22(14)
C2 C3 C4 120.00(13)
C8 C7 C6 120.65(16)
C14 C13 C12 120.65(13)
C3 C2 C1 119.85(13)
C17 C16 C15 121.27(14)
C16 C17 C12 121.00(13)
C13 C14 C15 121.54(13)
C5 C6 C7 120.14(16)
C6 C5 C4 120.78(16)
C16 C15 C14 117.66(14)
C16 C15 C18 121.39(15)
C14 C15 C18 120.95(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N2 C11 1.3971(16)
N2 C19 1.4002(17)
N1 C1 1.3318(17)
N1 C9 1.3697(18)
C1 C2 1.4259(19)
C1 C10 1.457(2)
C22 F2 1.3438(16)
C22 C23 1.376(2)
C22 C21 1.378(2)
C4 C5 1.416(2)
C4 C9 1.415(2)
C4 C3 1.420(2)
C12 C17 1.395(2)
C12 C13 1.3996(18)
C12 C11 1.4844(19)
C20 C21 1.3781(19)
C20 C19 1.3937(19)
C19 C24 1.4005(18)
C21 F1 1.3517(17)
C9 C8 1.410(2)
C23 F3 1.3481(15)
C23 C24 1.374(2)
C11 C10 1.3555(19)
C8 C7 1.371(2)
C3 C2 1.358(2)
C7 C6 1.404(3)
C13 C14 1.384(2)
C16 C17 1.385(2)
C16 C15 1.392(2)
C14 C15 1.392(2)
C18 C15 1.508(2)
C6 C5 1.367(3)
