#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:04:44 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223927 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/05/7700572.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_7700572
loop_
_publ_author_name
'Qin, Lu'
'Zhang, Yue'
'Chao, Jianbin'
'Cheng, Jianhua'
'Chen, Xia'
_publ_section_title
;
 Four- and five-coordinate aluminum complexes supported by N,O-bidentate
 β-pyrazylenolate ligands: synthesis, structure and application in ROP of
 ε-caprolactone and lactide.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12315
_journal_page_last               12325
_journal_paper_doi               10.1039/c9dt02330e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C15 H17 Al N2 O'
_chemical_formula_weight         268.29
_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   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-26 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.341(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.5229(7)
_cell_length_b                   20.9439(13)
_cell_length_c                   13.8001(9)
_cell_measurement_reflns_used    15691
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.2775
_cell_measurement_theta_min      2.897
_cell_volume                     2886.9(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26815
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.268
_diffrn_reflns_theta_min         2.818
_exptl_absorpt_coefficient_mu    0.134
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0470
_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)+(0.0462P)²+1.7063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5729
_reflns_number_total             7079
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02330e2.cif
_cod_data_source_block           1_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7700568--7700573.cif.'
_cod_database_code               7700572
_shelx_shelxl_version_number     2016/6
_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Al1 Al -0.13523(5) 0.10716(2) 0.68064(4) 0.03510(13) Uani 1 1 d . .
Al2 Al 0.62500(5) 0.95940(2) 0.80732(4) 0.03261(12) Uani 1 1 d . .
C4 C 0.09845(13) 0.12990(7) 0.61535(10) 0.0260(3) Uani 1 1 d . .
C21 C 0.37178(14) 1.00114(7) 0.86925(11) 0.0276(3) Uani 1 1 d . .
H21 H 0.288412 1.015835 0.873753 0.033 Uiso 1 1 calc R U
C23 C 0.42986(15) 1.11605(7) 0.85854(10) 0.0284(3) Uani 1 1 d . .
C6 C 0.12015(14) 0.06238(7) 0.62538(11) 0.0285(3) Uani 1 1 d . .
H6 H 0.205062 0.047183 0.625027 0.034 Uiso 1 1 calc R U
C7 C 0.03051(14) 0.01774(7) 0.63541(11) 0.0279(3) Uani 1 1 d . .
C22 C 0.45928(14) 1.04659(6) 0.85865(10) 0.0255(3) Uani 1 1 d . .
C19 C 0.39290(13) 0.93351(7) 0.87428(10) 0.0258(3) Uani 1 1 d . .
C1 C -0.02878(17) 0.22095(7) 0.61639(13) 0.0389(4) Uani 1 1 d . .
H1 H -0.106277 0.240353 0.624725 0.047 Uiso 1 1 calc R U
C18 C 0.30085(15) 0.89128(7) 0.89967(10) 0.0317(3) Uani 1 1 d . .
C8 C 0.05962(15) -0.05170(7) 0.63873(10) 0.0298(3) Uani 1 1 d . .
C9 C 0.17306(18) -0.07642(8) 0.62023(13) 0.0406(4) Uani 1 1 d . .
H9 H 0.233684 -0.048379 0.603130 0.049 Uiso 1 1 calc R U
C13 C -0.02871(18) -0.09398(8) 0.66193(12) 0.0395(4) Uani 1 1 d . .
H13 H -0.107284 -0.078227 0.673624 0.047 Uiso 1 1 calc R U
C5 C 0.31373(16) 0.14324(9) 0.56990(14) 0.0424(4) Uani 1 1 d . .
H5A H 0.364961 0.177682 0.551593 0.064 Uiso 1 1 calc R U
H5B H 0.286797 0.112133 0.514102 0.064 Uiso 1 1 calc R U
H5C H 0.369374 0.122084 0.632139 0.064 Uiso 1 1 calc R U
C3 C 0.19175(15) 0.17045(8) 0.58801(11) 0.0315(3) Uani 1 1 d . .
C17 C 0.4276(2) 0.80545(8) 0.88659(15) 0.0474(4) Uani 1 1 d . .
H17 H 0.442195 0.760631 0.890515 0.057 Uiso 1 1 calc R U
C24 C 0.31352(18) 1.13966(8) 0.87336(14) 0.0413(4) Uani 1 1 d . .
H24 H 0.250167 1.110780 0.884916 0.050 Uiso 1 1 calc R U
C28 C 0.52107(18) 1.15944(8) 0.84202(13) 0.0388(4) Uani 1 1 d . .
H28 H 0.601380 1.144433 0.832279 0.047 Uiso 1 1 calc R U
C30 C 0.5692(2) 0.95267(11) 0.65859(15) 0.0550(5) Uani 1 1 d . .
H30A H 0.487523 0.977752 0.629001 0.083 Uiso 1 1 calc R U
H30B H 0.551621 0.907828 0.638546 0.083 Uiso 1 1 calc R U
H30C H 0.640420 0.969041 0.633651 0.083 Uiso 1 1 calc R U
C20 C 0.18171(17) 0.91690(9) 0.92391(13) 0.0427(4) Uani 1 1 d . .
H20A H 0.130165 0.881389 0.938859 0.064 Uiso 1 1 calc R U
H20B H 0.125263 0.941028 0.865275 0.064 Uiso 1 1 calc R U
H20C H 0.211611 0.945082 0.983483 0.064 Uiso 1 1 calc R U
C11 C 0.1105(2) -0.18277(9) 0.65071(15) 0.0569(6) Uani 1 1 d . .
H11 H 0.128028 -0.227348 0.655347 0.068 Uiso 1 1 calc R U
C16 C 0.51836(18) 0.84367(8) 0.86338(14) 0.0413(4) Uani 1 1 d . .
H16 H 0.595355 0.825206 0.852740 0.050 Uiso 1 1 calc R U
C2 C 0.06240(19) 0.25757(8) 0.59035(15) 0.0456(4) Uani 1 1 d . .
H2 H 0.046981 0.302198 0.581369 0.055 Uiso 1 1 calc R U
C29 C 0.80696(18) 0.93444(10) 0.88486(17) 0.0531(5) Uani 1 1 d . .
H29A H 0.868496 0.969521 0.884646 0.080 Uiso 1 1 calc R U
H29B H 0.832435 0.896545 0.853621 0.080 Uiso 1 1 calc R U
H29C H 0.811472 0.924698 0.955325 0.080 Uiso 1 1 calc R U
C15 C -0.31885(18) 0.13044(10) 0.60455(17) 0.0541(5) Uani 1 1 d . .
H15A H -0.362871 0.094476 0.561613 0.081 Uiso 1 1 calc R U
H15B H -0.318500 0.167546 0.561365 0.081 Uiso 1 1 calc R U
H15C H -0.367520 0.141020 0.652405 0.081 Uiso 1 1 calc R U
C14 C -0.0772(2) 0.11682(12) 0.82895(16) 0.0606(5) Uani 1 1 d . .
H14A H -0.149323 0.103208 0.855140 0.091 Uiso 1 1 calc R U
H14B H -0.055451 0.161684 0.846751 0.091 Uiso 1 1 calc R U
H14C H 0.002252 0.090406 0.859347 0.091 Uiso 1 1 calc R U
C25 C 0.2891(2) 1.20488(9) 0.87143(16) 0.0557(5) Uani 1 1 d . .
H25 H 0.209656 1.220298 0.882143 0.067 Uiso 1 1 calc R U
C27 C 0.4953(2) 1.22470(9) 0.83970(15) 0.0532(5) Uani 1 1 d . .
H27 H 0.557994 1.253957 0.828124 0.064 Uiso 1 1 calc R U
C12 C -0.0024(2) -0.15922(9) 0.66807(15) 0.0528(5) Uani 1 1 d . .
H12 H -0.062879 -0.187719 0.684383 0.063 Uiso 1 1 calc R U
C26 C 0.3792(2) 1.24718(9) 0.85410(16) 0.0581(5) Uani 1 1 d . .
H26 H 0.361818 1.291747 0.852032 0.070 Uiso 1 1 calc R U
C10 C 0.1980(2) -0.14159(9) 0.62660(15) 0.0528(5) Uani 1 1 d . .
H10 H 0.275758 -0.157857 0.614277 0.063 Uiso 1 1 calc R U
N3 N 0.50048(12) 0.90773(6) 0.85521(9) 0.0296(3) Uani 1 1 d . .
N1 N -0.01032(12) 0.15719(6) 0.63056(9) 0.0292(3) Uani 1 1 d . .
N2 N 0.17357(15) 0.23270(7) 0.57692(11) 0.0416(3) Uani 1 1 d . .
N4 N 0.31838(16) 0.82874(7) 0.90410(11) 0.0421(3) Uani 1 1 d . .
O2 O 0.57676(11) 1.03296(5) 0.84886(10) 0.0394(3) Uani 1 1 d . .
O1 O -0.08842(12) 0.03247(5) 0.64161(11) 0.0457(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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
O1 Al1 C15 112.34(8)
O1 Al1 C14 112.60(9)
C15 Al1 C14 117.95(10)
O1 Al1 N1 94.76(5)
C15 Al1 N1 109.63(8)
C14 Al1 N1 106.84(8)
O2 Al2 C29 112.80(8)
O2 Al2 C30 112.35(8)
C29 Al2 C30 118.44(10)
O2 Al2 N3 94.62(5)
C29 Al2 N3 108.13(8)
C30 Al2 N3 107.54(8)
N1 C4 C6 121.26(12)
N1 C4 C3 118.20(13)
C6 C4 C3 120.54(13)
C22 C21 C19 126.57(13)
C28 C23 C24 118.37(14)
C28 C23 C22 119.01(14)
C24 C23 C22 122.62(14)
C7 C6 C4 126.26(13)
O1 C7 C6 123.15(13)
O1 C7 C8 114.74(13)
C6 C7 C8 122.11(13)
O2 C22 C21 123.17(13)
O2 C22 C23 114.45(12)
C21 C22 C23 122.38(13)
N3 C19 C21 120.80(12)
N3 C19 C18 118.18(13)
C21 C19 C18 121.02(13)
N1 C1 C2 120.82(15)
N4 C18 C19 121.83(15)
N4 C18 C20 117.39(14)
C19 C18 C20 120.78(14)
C13 C8 C9 118.50(15)
C13 C8 C7 118.96(14)
C9 C8 C7 122.54(14)
C10 C9 C8 120.58(18)
C12 C13 C8 120.27(18)
N2 C3 C4 121.92(14)
N2 C3 C5 117.25(14)
C4 C3 C5 120.83(14)
N4 C17 C16 122.32(16)
C25 C24 C23 120.80(18)
C23 C28 C27 120.38(17)
C12 C11 C10 119.83(17)
N3 C16 C17 120.89(16)
N2 C2 C1 122.23(16)
C26 C25 C24 120.28(19)
C26 C27 C28 120.42(18)
C11 C12 C13 120.54(19)
C25 C26 C27 119.75(17)
C11 C10 C9 120.3(2)
C19 N3 C16 118.82(13)
C19 N3 Al2 122.17(10)
C16 N3 Al2 118.89(11)
C4 N1 C1 118.93(13)
C4 N1 Al1 121.35(10)
C1 N1 Al1 119.61(11)
C3 N2 C2 117.85(14)
C18 N4 C17 117.91(14)
C22 O2 Al2 126.54(10)
C7 O1 Al1 125.89(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Al1 O1 1.7739(13)
Al1 C15 1.9486(19)
Al1 C14 1.953(2)
Al1 N1 1.9685(13)
Al2 O2 1.7728(12)
Al2 C29 1.9481(19)
Al2 C30 1.954(2)
Al2 N3 1.9672(13)
C4 N1 1.3535(18)
C4 C6 1.432(2)
C4 C3 1.4355(19)
C21 C22 1.3637(19)
C21 C19 1.4321(19)
C23 C28 1.392(2)
C23 C24 1.394(2)
C23 C22 1.4872(19)
C6 C7 1.366(2)
C7 O1 1.3176(18)
C7 C8 1.484(2)
C22 O2 1.3165(17)
C19 N3 1.3527(18)
C19 C18 1.4341(19)
C1 N1 1.3547(19)
C1 C2 1.362(2)
C18 N4 1.322(2)
C18 C20 1.495(2)
C8 C13 1.392(2)
C8 C9 1.396(2)
C9 C10 1.387(2)
C13 C12 1.391(2)
C5 C3 1.496(2)
C3 N2 1.320(2)
C17 N4 1.339(2)
C17 C16 1.359(2)
C24 C25 1.389(2)
C28 C27 1.392(2)
C11 C12 1.375(3)
C11 C10 1.377(3)
C16 N3 1.3545(19)
C2 N2 1.346(2)
C25 C26 1.373(3)
C27 C26 1.380(3)
