#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:27:23 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229867 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/59/7045993.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_7045993
loop_
_publ_author_name
'Ye, Cai-Ping'
'Xu, Gan'
'Wang, Zheng'
'Han, Jie'
'Xue, Lian'
'Cao, Fu-Yu'
'Zhang, Qi'
'Yang, Lin-Feng'
'Lin, Li-Zhou'
'Chen, Xu-Dong'
_publ_section_title
;
 Design and synthesis of functionalized coordination polymers as
 recyclable heterogeneous photocatalysts.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6470
_journal_page_last               6478
_journal_paper_doi               10.1039/c8dt00902c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C16 H12 Ni O9, 2(H2 O)'
_chemical_formula_sum            'C16 H16 Ni O11'
_chemical_formula_weight         443.00
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-02 deposited with the CCDC.
2018-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.258(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6610(18)
_cell_length_b                   21.487(4)
_cell_length_c                   7.6743(13)
_cell_measurement_reflns_used    4742
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.316
_cell_measurement_theta_min      2.724
_cell_volume                     1717.9(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12057
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.316
_diffrn_reflns_theta_min         1.895
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0704 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.8219.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       irregular
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0317
_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)+(0.0390P)²+1.7090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2602
_reflns_number_total             3121
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00902c2.cif
_cod_data_source_block           ycp-29
_cod_depositor_comments
'Adding full bibliography for 7045991--7045995.cif.'
_cod_database_code               7045993
_shelx_shelxl_version_number     2016/4
_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) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
C1 C 0.6453(2) 0.33065(11) 0.6591(3) 0.0173(5) Uani 1 1 d .
C2 C 0.5933(2) 0.27909(12) 0.5598(3) 0.0232(6) Uani 1 1 d .
H2 H 0.643807 0.243975 0.556731 0.028 Uiso 1 1 calc R
C3 C 0.4669(2) 0.27947(12) 0.4652(3) 0.0247(6) Uani 1 1 d .
H3 H 0.434129 0.244947 0.397584 0.030 Uiso 1 1 calc R
C4 C 0.3890(2) 0.33092(12) 0.4707(3) 0.0184(5) Uani 1 1 d .
C5 C 0.3321(3) 0.54120(13) 0.7137(4) 0.0304(6) Uani 1 1 d .
H5 H 0.244599 0.539528 0.664445 0.036 Uiso 1 1 calc R
C6 C 0.3838(3) 0.59298(13) 0.8113(4) 0.0349(7) Uani 1 1 d .
H6 H 0.330888 0.625765 0.828761 0.042 Uiso 1 1 calc R
C7 C 0.5144(3) 0.59573(13) 0.8827(4) 0.0328(7) Uani 1 1 d .
H7 H 0.548801 0.630674 0.947004 0.039 Uiso 1 1 calc R
C8 C 0.5940(3) 0.54733(12) 0.8596(3) 0.0262(6) Uani 1 1 d .
H8 H 0.681582 0.549766 0.907900 0.031 Uiso 1 1 calc R
C9 C 0.6292(2) 0.44344(12) 0.7373(3) 0.0199(5) Uani 1 1 d .
C10 C 0.3546(2) 0.43686(12) 0.5848(3) 0.0207(5) Uani 1 1 d .
C11 C 0.4109(2) 0.49194(12) 0.6895(3) 0.0220(5) Uani 1 1 d .
C12 C 0.5433(2) 0.49469(11) 0.7638(3) 0.0200(5) Uani 1 1 d .
C13 C 0.5697(2) 0.38399(11) 0.6588(3) 0.0161(5) Uani 1 1 d .
C14 C 0.4397(2) 0.38328(11) 0.5696(3) 0.0172(5) Uani 1 1 d .
C15 C 0.2526(2) 0.32569(11) 0.3637(3) 0.0189(5) Uani 1 1 d .
C16 C 0.7774(2) 0.32307(11) 0.7757(3) 0.0172(5) Uani 1 1 d .
Ni1 Ni 0.01922(3) 0.24835(2) 0.31939(4) 0.01445(11) Uani 1 1 d .
O1 O 0.23996(18) 0.43446(9) 0.5188(3) 0.0389(5) Uani 1 1 d .
O2 O 0.74552(17) 0.45007(9) 0.7711(3) 0.0322(5) Uani 1 1 d .
O3 O 0.79089(17) 0.33076(9) 0.9379(2) 0.0259(4) Uani 1 1 d .
O4 O 0.86502(16) 0.30434(9) 0.6980(2) 0.0228(4) Uani 1 1 d .
O5 O 0.22948(18) 0.34259(10) 0.2066(2) 0.0334(5) Uani 1 1 d .
O6 O 0.17416(16) 0.29855(9) 0.4415(2) 0.0234(4) Uani 1 1 d .
O7 O 0.01694(15) 0.21140(8) 0.56996(19) 0.0153(3) Uani 1 1 d .
H7A H 0.077969 0.184811 0.600164 0.023 Uiso 1 1 d R
H7B H -0.049161 0.188521 0.530454 0.023 Uiso 1 1 d R
O8 O 0.14210(17) 0.17875(9) 0.2756(2) 0.0272(4) Uani 1 1 d .
H8A H 0.153926 0.181346 0.168447 0.041 Uiso 1 1 d R
H8B H 0.116536 0.142076 0.296547 0.041 Uiso 1 1 d R
O9 O -0.10450(17) 0.31830(9) 0.3602(2) 0.0260(4) Uani 1 1 d .
H9A H -0.123664 0.319438 0.463477 0.039 Uiso 1 1 d R
H9B H -0.084424 0.356218 0.342757 0.039 Uiso 1 1 d R
O10 O -0.0034(2) 0.43462(12) 0.2580(4) 0.0629(7) Uani 1 1 d .
H10A H 0.073089 0.436015 0.322653 0.094 Uiso 1 1 d R
H10B H 0.022728 0.428905 0.160603 0.094 Uiso 1 1 d R
O11 O 0.0244(3) 0.06811(12) 0.3635(4) 0.0708(8) Uani 1 1 d .
H11A H 0.033818 0.032935 0.314303 0.106 Uiso 1 1 d R
H11B H -0.057002 0.066645 0.321614 0.106 Uiso 1 1 d R
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'
Ni Ni 0.3393 1.1124 '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'
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
C2 C1 C13 119.3(2) . .
C2 C1 C16 116.9(2) . .
C13 C1 C16 123.6(2) . .
C1 C2 H2 119.6 . .
C3 C2 C1 120.7(2) . .
C3 C2 H2 119.6 . .
C2 C3 H3 119.7 . .
C2 C3 C4 120.6(2) . .
C4 C3 H3 119.7 . .
C3 C4 C14 119.5(2) . .
C3 C4 C15 115.8(2) . .
C14 C4 C15 124.7(2) . .
C6 C5 H5 120.0 . .
C11 C5 H5 120.0 . .
C11 C5 C6 120.1(3) . .
C5 C6 H6 120.1 . .
C7 C6 C5 119.9(3) . .
C7 C6 H6 120.1 . .
C6 C7 H7 119.6 . .
C8 C7 C6 120.8(3) . .
C8 C7 H7 119.6 . .
C7 C8 H8 120.0 . .
C7 C8 C12 120.0(3) . .
C12 C8 H8 120.0 . .
C12 C9 C13 118.1(2) . .
O2 C9 C12 121.1(2) . .
O2 C9 C13 120.7(2) . .
C11 C10 C14 118.5(2) . .
O1 C10 C11 120.8(2) . .
O1 C10 C14 120.6(2) . .
C5 C11 C10 119.6(2) . .
C5 C11 C12 119.8(2) . .
C12 C11 C10 120.6(2) . .
C8 C12 C9 119.7(2) . .
C8 C12 C11 119.4(2) . .
C11 C12 C9 120.8(2) . .
C1 C13 C9 120.3(2) . .
C1 C13 C14 119.9(2) . .
C14 C13 C9 119.6(2) . .
C4 C14 C10 119.6(2) . .
C4 C14 C13 119.9(2) . .
C13 C14 C10 120.5(2) . .
O5 C15 C4 118.6(2) . .
O5 C15 O6 125.5(2) . .
O6 C15 C4 115.6(2) . .
O3 C16 C1 118.6(2) . .
O3 C16 O4 125.0(2) . .
O4 C16 C1 116.2(2) . .
O4 Ni1 O7 92.49(6) 4_465 .
O4 Ni1 O7 87.72(6) 4_465 4_565
O4 Ni1 O8 90.08(7) 4_465 .
O4 Ni1 O9 89.68(7) 4_465 .
O6 Ni1 O4 178.61(7) . 4_465
O6 Ni1 O7 86.80(6) . .
O6 Ni1 O7 93.04(6) . 4_565
O6 Ni1 O8 88.73(8) . .
O6 Ni1 O9 91.52(8) . .
O7 Ni1 O7 177.62(6) . 4_565
O8 Ni1 O7 92.01(7) . 4_565
O8 Ni1 O7 90.36(7) . .
O8 Ni1 O9 179.35(7) . .
O9 Ni1 O7 90.25(7) . .
O9 Ni1 O7 87.37(7) . 4_565
C16 O4 Ni1 123.95(15) . 4_666
C15 O6 Ni1 125.50(15) . .
Ni1 O7 Ni1 133.23(8) . 4_566
Ni1 O7 H7A 110.2 . .
Ni1 O7 H7A 99.6 4_566 .
Ni1 O7 H7B 93.5 . .
Ni1 O7 H7B 114.1 4_566 .
H7A O7 H7B 103.4 . .
Ni1 O8 H8A 109.6 . .
Ni1 O8 H8B 113.4 . .
H8A O8 H8B 110.8 . .
Ni1 O9 H9A 116.4 . .
Ni1 O9 H9B 118.5 . .
H9A O9 H9B 103.4 . .
H10A O10 H10B 93.7 . .
H11A O11 H11B 90.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.391(3) .
C1 C13 1.401(3) .
C1 C16 1.509(3) .
C2 H2 0.9300 .
C2 C3 1.388(4) .
C3 H3 0.9300 .
C3 C4 1.389(4) .
C4 C14 1.400(3) .
C4 C15 1.515(3) .
C5 H5 0.9300 .
C5 C6 1.388(4) .
C5 C11 1.388(4) .
C6 H6 0.9300 .
C6 C7 1.385(4) .
C7 H7 0.9300 .
C7 C8 1.377(4) .
C8 H8 0.9300 .
C8 C12 1.394(3) .
C9 C12 1.474(3) .
C9 C13 1.495(3) .
C9 O2 1.220(3) .
C10 C11 1.484(4) .
C10 C14 1.485(3) .
C10 O1 1.221(3) .
C11 C12 1.407(4) .
C13 C14 1.410(3) .
C15 O5 1.233(3) .
C15 O6 1.268(3) .
C16 O3 1.234(3) .
C16 O4 1.275(3) .
Ni1 O4 2.0497(16) 4_465
Ni1 O6 2.0282(17) .
Ni1 O7 2.0853(15) .
Ni1 O7 2.0959(15) 4_565
Ni1 O8 2.0621(18) .
Ni1 O9 2.0670(18) .
O4 Ni1 2.0497(16) 4_666
O7 Ni1 2.0959(15) 4_566
O7 H7A 0.8599 .
O7 H7B 0.8599 .
O8 H8A 0.8600 .
O8 H8B 0.8599 .
O9 H9A 0.8600 .
O9 H9B 0.8601 .
O10 H10A 0.8599 .
O10 H10B 0.8599 .
O11 H11A 0.8601 .
O11 H11B 0.8600 .
