#------------------------------------------------------------------------------
#$Date: 2020-10-06 12:19:37 +0200 (mar 06 de oct de 2020) $
#$Revision: 257796 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/96/7059680.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_7059680
loop_
_publ_author_name
'Nakane, Tomohiro'
'Aoyagi, Shinobu'
'Fujita, Wataru'
_publ_section_title
;
 Magnetic and thermal studies of a coordination polymer:
 bis(glycolato)nickel(ii)
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10519
_journal_page_last               10524
_journal_paper_doi               10.1039/D0NJ01450H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C4 H6 Ni O6'
_chemical_formula_weight         208.80
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2020-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.413(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.1389(17)
_cell_length_b                   7.650(2)
_cell_length_c                   8.618(3)
_cell_measurement_reflns_used    1057
_cell_measurement_temperature    299(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.60
_cell_volume                     326.61(18)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299(1)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3560
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.621
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_description       prism
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0209
_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)+(0.0316P)²+0.0950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                681
_reflns_number_total             740
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj01450h1.cif
_cod_data_source_block           200422f1a_299k
_cod_depositor_comments
;Adding full bibliography for 7059680--7059681.cif.

 Adding full bibliography for 7059680--7059681.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7059680
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.590
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.500000 0.500000 0.500000 0.01241(14) Uani 1 2 d S . P . .
O2 O 0.4751(2) 0.34959(16) 0.68726(15) 0.0178(3) Uani 1 1 d . . . . .
O3 O 0.7728(3) 0.31001(17) 0.48732(15) 0.0186(3) Uani 1 1 d . . . . .
H3 H 0.929(7) 0.322(4) 0.445(4) 0.061(9) Uiso 1 1 d . . . . .
O4 O 0.6800(2) 0.14460(18) 0.85542(15) 0.0200(3) Uani 1 1 d . . . . .
C5 C 0.6545(3) 0.2359(2) 0.7300(2) 0.0153(4) Uani 1 1 d . . . . .
C6 C 0.8479(4) 0.2046(3) 0.6275(3) 0.0283(5) Uani 1 1 d . . . . .
H6A H 1.013(6) 0.242(4) 0.695(3) 0.048(8) Uiso 1 1 d . . . . .
H6B H 0.835(6) 0.067(4) 0.591(4) 0.056(8) Uiso 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'
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
_geom_angle_publ_flag
O2 Ni1 O2 180.00(9) . 3_666 ?
O2 Ni1 O3 99.96(5) . 3_666 ?
O2 Ni1 O3 80.04(5) 3_666 3_666 ?
O2 Ni1 O3 80.04(5) . . ?
O2 Ni1 O3 99.96(5) 3_666 . ?
O3 Ni1 O3 180.0 3_666 . ?
O2 Ni1 O4 88.16(5) . 4_565 ?
O2 Ni1 O4 91.84(5) 3_666 4_565 ?
O3 Ni1 O4 88.06(6) 3_666 4_565 ?
O3 Ni1 O4 91.94(6) . 4_565 ?
O2 Ni1 O4 91.84(5) . 2_656 ?
O2 Ni1 O4 88.16(5) 3_666 2_656 ?
O3 Ni1 O4 91.94(6) 3_666 2_656 ?
O3 Ni1 O4 88.06(6) . 2_656 ?
O4 Ni1 O4 180.0 4_565 2_656 ?
C5 O2 Ni1 115.77(11) . . ?
C6 O3 Ni1 113.23(11) . . ?
C6 O3 H3 108(2) . . ?
Ni1 O3 H3 126.8(19) . . ?
C5 O4 Ni1 133.37(12) . 2_646 ?
O2 C5 O4 122.50(16) . . ?
O2 C5 C6 119.04(15) . . ?
O4 C5 C6 118.46(16) . . ?
O3 C6 C5 109.57(15) . . ?
O3 C6 H6A 110.4(18) . . ?
C5 C6 H6A 102.7(18) . . ?
O3 C6 H6B 108.8(18) . . ?
C5 C6 H6B 108.7(17) . . ?
H6A C6 H6B 116(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.0137(13) . ?
Ni1 O2 2.0137(13) 3_666 ?
Ni1 O3 2.0423(13) 3_666 ?
Ni1 O3 2.0423(13) . ?
Ni1 O4 2.0956(13) 4_565 ?
Ni1 O4 2.0956(13) 2_656 ?
O2 C5 1.250(2) . ?
O3 C6 1.418(2) . ?
O3 H3 0.97(3) . ?
O4 C5 1.264(2) . ?
C5 C6 1.514(3) . ?
C6 H6A 0.94(3) . ?
C6 H6B 1.09(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O4 0.97(3) 1.69(3) 2.6563(19) 174(3) 4_665 yes
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C5 O4 172.60(13) . . . . ?
Ni1 O2 C5 C6 -8.0(2) . . . . ?
Ni1 O4 C5 O2 -159.60(13) 2_646 . . . ?
Ni1 O4 C5 C6 21.0(3) 2_646 . . . ?
Ni1 O3 C6 C5 13.4(2) . . . . ?
O2 C5 C6 O3 -3.9(3) . . . . ?
O4 C5 C6 O3 175.58(16) . . . . ?
