#------------------------------------------------------------------------------
#$Date: 2022-05-20 04:04:56 +0300 (Fri, 20 May 2022) $
#$Revision: 275568 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/49/7244964.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_7244964
loop_
_publ_author_name
'Ma, Huan'
'Liu, Zhiyong'
'Liu, Zhihong'
_publ_section_title
;
 The formation mechanism of fibrous metal oxalate prepared by ammonia
 coordination method
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              15251
_journal_page_last               15260
_journal_paper_doi               10.1039/D2RA00605G
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C2 H6 N2 Ni O4'
_chemical_formula_weight         180.80
_chemical_name_systematic        'nickel ammine oxalate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-11-21 deposited with the CCDC.	2022-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.295(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7631(15)
_cell_length_b                   5.4109(8)
_cell_length_c                   4.9961(7)
_cell_measurement_reflns_used    937
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.81
_cell_volume                     289.21(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0078
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            973
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         3.809
_exptl_absorpt_coefficient_mu    3.296
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_description       block
_exptl_crystal_F_000             184
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0140
_refine_ls_R_factor_gt           0.0140
_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)+(0.0197P)²+0.2112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                371
_reflns_number_total             371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra00605g2.cif
_cod_data_source_block           c2m
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7244964
_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. 
;
_shelx_estimated_absorpt_t_min   0.505
_shelx_estimated_absorpt_t_max   0.559
_shelx_res_file
; 
TITL c2m in C2/m 
    c2m.res 
    created by SHELXL-2016/6 at 17:05:27 on 15-Jul-2018 
CELL 0.71073  10.76310   5.41090   4.99610  90.0000  96.2953  90.0000 
ZERR    2.00   0.00150   0.00080   0.00070   0.0000   0.0056   0.0000 
LATT 7 
SYMM -X, Y, -Z 
SFAC C  H  N  O  Ni 
UNIT 4  12  4  8  2 
L.S. 4 
ACTA 
BOND $h 
FMAP 2 
PLAN 4 
size 0.20 0.22 0.24 
conf 
TEMP 23.000 
WGHT    0.019700    0.211200 
FVAR       0.33580 
MOLE 1 
NI1   5    0.000000    1.000000    0.000000    10.25000    0.02168    0.01043 = 
         0.02166    0.00000    0.00737    0.00000 
O1    4   -0.087543    0.705787    0.173022    11.00000    0.02777    0.01325 = 
         0.02851   -0.00110    0.01332    0.00074 
N1    3    0.141102    1.000000    0.318632    10.50000    0.02535    0.02608 = 
         0.02571    0.00000    0.00457    0.00000 
AFIX 137 
H2A   2    0.121461    1.104445    0.445023    10.50000   -1.50000 
H2B   2    0.212575    1.047049    0.259924    10.50000   -1.50000 
H2C   2    0.149758    0.848506    0.387538    10.50000   -1.50000 
AFIX   0 
C1    1   -0.050909    0.500000    0.100726    10.50000    0.01842    0.01579 = 
         0.01956    0.00000    0.00632    0.00000 
HKLF 4 
  
  
  
  
REM  c2m in C2/m 
REM R1 =  0.0140 for     371 Fo > 4sig(Fo)  and  0.0140 for all     371 data 
REM     27 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0171      0.2175 
  
REM Highest difference peak  0.483,  deepest hole -0.214,  1-sigma level  0.052 
Q1    1   0.0000  0.5000  0.0000  10.25000  0.05    0.48 
Q2    1  -0.0079  1.0000  0.1619  10.50000  0.05    0.29 
Q3    1   0.0340  1.0996  0.1320  11.00000  0.05    0.22 
Q4    1   0.0825  1.0000  0.2121  10.50000  0.05    0.21 
;
_shelx_res_checksum              19547
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.000000 1.000000 0.000000 0.01755(11) Uani 1 4 d S T P . .
O1 O -0.08754(8) 0.70579(16) 0.17302(17) 0.0224(2) Uani 1 1 d . . . . .
N1 N 0.14110(14) 1.000000 0.3186(3) 0.0256(3) Uani 1 2 d S T P . .
H2A H 0.121461 1.104445 0.445023 0.038 Uiso 0.5 1 calc R U P . .
H2B H 0.212575 1.047049 0.259924 0.038 Uiso 0.5 1 calc R U P . .
H2C H 0.149758 0.848506 0.387538 0.038 Uiso 0.5 1 calc R U P . .
C1 C -0.05091(15) 0.500000 0.1007(3) 0.0176(3) Uani 1 2 d S T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02168(17) 0.01043(16) 0.02166(17) 0.000 0.00737(11) 0.000
O1 0.0278(4) 0.0133(4) 0.0285(4) -0.0011(3) 0.0133(3) 0.0007(3)
N1 0.0253(7) 0.0261(8) 0.0257(7) 0.000 0.0046(6) 0.000
C1 0.0184(7) 0.0158(8) 0.0196(7) 0.000 0.0063(6) 0.000
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'
Ni Ni 0.3393 1.1124 '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
N1 Ni1 N1 180.0 5_575 . ?
N1 Ni1 O1 90.45(4) 5_575 5_575 ?
N1 Ni1 O1 89.55(4) . 5_575 ?
N1 Ni1 O1 89.55(4) 5_575 6_575 ?
N1 Ni1 O1 90.45(4) . 6_575 ?
O1 Ni1 O1 80.46(4) 5_575 6_575 ?
N1 Ni1 O1 90.45(4) 5_575 2 ?
N1 Ni1 O1 89.55(4) . 2 ?
O1 Ni1 O1 99.54(4) 5_575 2 ?
O1 Ni1 O1 180.0 6_575 2 ?
N1 Ni1 O1 89.55(4) 5_575 . ?
N1 Ni1 O1 90.45(4) . . ?
O1 Ni1 O1 180.0 5_575 . ?
O1 Ni1 O1 99.54(4) 6_575 . ?
O1 Ni1 O1 80.46(4) 2 . ?
C1 O1 Ni1 112.94(7) . . ?
Ni1 N1 H2A 109.5 . . ?
Ni1 N1 H2B 109.5 . . ?
H2A N1 H2B 109.5 . . ?
Ni1 N1 H2C 109.5 . . ?
H2A N1 H2C 109.5 . . ?
H2B N1 H2C 109.5 . . ?
Ni1 N1 H2A 109.5(4) . 6_575 ?
H2A N1 H2A 78.8 . 6_575 ?
H2B N1 H2A 134.2 . 6_575 ?
H2C N1 H2A 33.2 . 6_575 ?
Ni1 N1 H2B 109.5(2) . 6_575 ?
H2A N1 H2B 134.2 . 6_575 ?
H2B N1 H2B 33.2 . 6_575 ?
H2C N1 H2B 78.8 . 6_575 ?
H2A N1 H2B 109.5 6_575 6_575 ?
Ni1 N1 H2C 109.47(17) . 6_575 ?
H2A N1 H2C 33.2 . 6_575 ?
H2B N1 H2C 78.8 . 6_575 ?
H2C N1 H2C 134.2 . 6_575 ?
H2A N1 H2C 109.5 6_575 6_575 ?
H2B N1 H2C 109.5 6_575 6_575 ?
O1 C1 O1 126.34(14) 6_565 . ?
O1 C1 C1 116.83(7) 6_565 5_565 ?
O1 C1 C1 116.83(7) . 5_565 ?
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 N1 2.0761(15) 5_575 ?
Ni1 N1 2.0762(15) . ?
Ni1 O1 2.0852(8) 5_575 ?
Ni1 O1 2.0852(8) 6_575 ?
Ni1 O1 2.0852(8) 2 ?
Ni1 O1 2.0852(8) . ?
O1 C1 1.2478(11) . ?
N1 H2A 0.8900 . ?
N1 H2B 0.8900 . ?
N1 H2C 0.8900 . ?
N1 H2A 0.890(18) 6_575 ?
N1 H2B 0.890(10) 6_575 ?
N1 H2C 0.890(7) 6_575 ?
C1 C1 1.567(3) 5_565 ?
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 O1 C1 O1 -179.97(12) . . . 6_565 ?
Ni1 O1 C1 C1 0.0(2) . . . 5_565 ?
