#------------------------------------------------------------------------------
#$Date: 2019-11-05 01:55:56 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223252 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/49/7234947.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_7234947
loop_
_publ_author_name
'Chai, Juan'
'Zhang, Ping'
'Shi, Xiangxiang'
'Sun, Jing'
'Wang, Li'
'Fan, Yong'
_publ_section_title
;
 Three helical chain-based 3D coordination polymers: solvent-induced
 syntheses, tunable structures and catalytic properties for the Strecker
 reaction
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5440
_journal_paper_doi               10.1039/C9CE00972H
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C8 H5 N O5 Sc'
_chemical_formula_weight         240.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1q71vv
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-30 deposited with the CCDC.	2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.401(3)
_cell_length_b                   22.401(3)
_cell_length_c                   11.964(2)
_cell_measurement_reflns_used    27581
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.22
_cell_volume                     6003.6(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  IP
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22423
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.216
_exptl_absorpt_coefficient_mu    0.490
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1402
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.362
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0649
_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)+(0.1072P)²+21.4243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1286
_reflns_number_total             1402
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00972h2.cif
_cod_data_source_block           c1_sq
_cod_original_cell_volume        6003.6(19)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               7234947
_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'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-x+1/2, y, -z+1/2'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-x+1, y+1/2, -z+1'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'x-1/2, -y, z-1/2'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'x, -y+1/2, z'
'y+1/4, x+1/4, z-1/4'
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
_atom_site_refinement_flags_occupancy
Sc1 Sc 0.7500 0.56580(4) 1.2500 0.0185(4) Uani 1 2 d S T P
O1 O 0.74707(11) 0.50293(11) 1.3750 0.0272(8) Uani 1 2 d S T P
O2 O 0.75966(14) 0.63630(11) 1.1298(2) 0.0388(8) Uani 1 1 d . . .
O3 O 0.65682(12) 0.56343(14) 1.2450(2) 0.0407(8) Uani 1 1 d . . .
N1 N 0.8367(7) 0.7500 0.6977(8) 0.153(5) Uani 1 2 d S TU P
H1A H 0.8419 0.7168 0.6631 0.183 Uiso 0.5 1 d R U P
H1B H 0.8395 0.7832 0.6621 0.183 Uiso 0.5 1 d R U P
C1 C 0.7892(2) 0.63783(17) 1.0405(4) 0.0393(10) Uani 1 1 d . . .
C2 C 0.7973(3) 0.6966(2) 0.9829(4) 0.071(2) Uani 1 1 d . . .
C3 C 0.8148(4) 0.6963(3) 0.8714(6) 0.101(3) Uani 1 1 d . U .
H3 H 0.8235 0.6604 0.8360 0.121 Uiso 1 1 calc R U .
C4 C 0.8192(6) 0.7500 0.8127(9) 0.103(3) Uani 1 2 d S TU P
C5 C 0.7851(3) 0.7500 1.0364(5) 0.0456(17) Uani 1 2 d S T P
H5 H 0.7688 0.7500 1.1079 0.055 Uiso 1 2 calc R U P
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'
Sc Sc 0.2519 0.3716 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Sc1 O1 93.50(11) 4_564 .
O1 Sc1 O3 89.64(11) 4_564 .
O1 Sc1 O3 88.37(10) . .
O1 Sc1 O3 88.36(10) 4_564 7_657
O1 Sc1 O3 89.64(11) . 7_657
O3 Sc1 O3 177.09(17) . 7_657
O1 Sc1 O2 90.78(10) 4_564 .
O1 Sc1 O2 174.09(9) . .
O3 Sc1 O2 95.76(11) . .
O3 Sc1 O2 86.39(12) 7_657 .
O1 Sc1 O2 174.09(9) 4_564 7_657
O1 Sc1 O2 90.78(10) . 7_657
O3 Sc1 O2 86.39(12) . 7_657
O3 Sc1 O2 95.76(11) 7_657 7_657
O2 Sc1 O2 85.27(15) . 7_657
Sc1 O1 Sc1 124.98(17) . 2_645
C1 O2 Sc1 130.0(3) . .
C1 O3 Sc1 142.3(3) 2_645 .
C4 N1 H1A 120.1 . .
C4 N1 H1B 119.8 . .
H1A N1 H1B 120.0 . .
O2 C1 O3 124.9(4) . 4_564
O2 C1 C2 118.6(3) . .
O3 C1 C2 116.5(4) 4_564 .
C5 C2 C3 120.3(5) . .
C5 C2 C1 121.5(4) . .
C3 C2 C1 118.1(4) . .
C2 C3 C4 119.9(6) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C3 C4 C3 118.9(9) . 31_565
C3 C4 N1 120.2(4) . .
C3 C4 N1 120.2(4) 31_565 .
C2 C5 C2 119.6(6) 31_565 .
C2 C5 H5 120.2 31_565 .
C2 C5 H5 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sc1 O1 2.0552(16) 4_564
Sc1 O1 2.0553(16) .
Sc1 O3 2.089(3) .
Sc1 O3 2.089(3) 7_657
Sc1 O2 2.147(3) .
Sc1 O2 2.147(3) 7_657
O1 Sc1 2.0553(16) 2_645
O2 C1 1.257(5) .
O3 C1 1.261(5) 2_645
N1 C4 1.430(13) .
N1 H1A 0.8601 .
N1 H1B 0.8601 .
C1 O3 1.261(5) 4_564
C1 C2 1.498(6) .
C2 C5 1.384(5) .
C2 C3 1.390(7) .
C3 C4 1.396(8) .
C3 H3 0.9300 .
C4 C3 1.396(8) 31_565
C5 C2 1.384(5) 31_565
C5 H5 0.9300 .
