#------------------------------------------------------------------------------
#$Date: 2019-04-13 01:00:53 +0300 (Sat, 13 Apr 2019) $
#$Revision: 214617 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/33/7123302.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_7123302
loop_
_publ_author_name
'Zhang, Wen-Da'
'Yan, Xiaodong'
'Li, Tao'
'Liu, Yong'
'Fu, Qiu-Ting'
'Gu, Zhi-Guo'
_publ_section_title
;
 Metal-organic layers derived metal hydroxide nanosheets for highly
 efficient oxygen evolution
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01808E
_journal_year                    2019
_chemical_formula_moiety         'C4 H4 Mn N4 Ni O2, 4(H2 O)'
_chemical_formula_sum            'C4 H12 Mn N4 Ni O6'
_chemical_formula_weight         325.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-21 deposited with the CCDC.    2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1445(9)
_cell_length_b                   14.1014(12)
_cell_length_c                   7.3111(5)
_cell_measurement_reflns_used    1513
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      3.36
_cell_volume                     1252.06(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0436
_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       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5588
_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         25.356
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.529
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1192
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0335
_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)+(0.0266P)²+0.5928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                867
_reflns_number_total             1192
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc01808e2.cif
_cod_data_source_block           1
_cod_database_code               7123302
_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.
;
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.843
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Ni1 Ni 0.56988(4) 0.2500 0.98877(7) 0.01049(16) Uani 1 2 d S T P
Mn2 Mn 0.5000 0.5000 0.5000 0.00969(18) Uani 1 2 d S . P
C1 C 0.5761(3) 0.3433(2) 0.8080(4) 0.0125(7) Uani 1 1 d . . .
C2 C 0.5452(3) 0.3426(2) 1.1660(4) 0.0141(8) Uani 1 1 d . . .
N1 N 0.5727(2) 0.4004(2) 0.6970(3) 0.0181(6) Uani 1 1 d . . .
N2 N 0.5267(2) 0.3989(2) 1.2750(4) 0.0203(7) Uani 1 1 d . . .
O1 O 0.33664(18) 0.43708(16) 0.5691(3) 0.0178(5) Uani 1 1 d . . .
H1A H 0.2803 0.4768 0.5561 0.053(14) Uiso 1 1 d R . .
H1B H 0.3259 0.3891 0.5011 0.064 Uiso 0.5 1 d R U P
H1C H 0.3382 0.4178 0.6793 0.064 Uiso 0.5 1 d R U P
O2 O 0.17894(19) 0.56815(17) 0.4560(3) 0.0234(6) Uani 1 1 d D . .
H2A H 0.1209(17) 0.566(2) 0.514(3) 0.028 Uiso 1 1 d D U .
H2B H 0.1642 0.5562 0.3452 0.028 Uiso 0.5 1 d R U P
H2C H 0.2082 0.6197 0.4680 0.028 Uiso 0.5 1 d R U P
O3 O 0.7887(3) 0.2500 0.0564(4) 0.0247(8) Uani 1 2 d DS T P
H3A H 0.785(3) 0.2500 0.167(3) 0.030 Uiso 1 2 d DS U P
H3D H 0.8017 0.1944 -0.0033 0.030 Uiso 0.5 1 d R U P
O4 O 0.7477(3) 0.2500 0.4413(5) 0.0282(9) Uani 1 2 d S T P
H4A H 0.6844 0.2500 0.4972 0.034 Uiso 1 2 d R U P
H4B H 0.7785 0.3030 0.4624 0.034 Uiso 0.5 1 d 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'
Mn Mn 0.3368 0.7283 '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
C2 Ni1 C2 88.96(19) 7_565 .
C2 Ni1 C1 173.05(15) 7_565 .
C2 Ni1 C1 90.26(13) . .
C2 Ni1 C1 90.26(13) 7_565 7_565
C2 Ni1 C1 173.05(15) . 7_565
C1 Ni1 C1 89.69(18) . 7_565
N1 Mn2 N1 180.0 . 5_666
N1 Mn2 N2 89.04(10) . 5_667
N1 Mn2 N2 90.96(10) 5_666 5_667
N1 Mn2 N2 90.96(10) . 1_554
N1 Mn2 N2 89.04(10) 5_666 1_554
N2 Mn2 N2 180.0 5_667 1_554
N1 Mn2 O1 87.39(10) . .
N1 Mn2 O1 92.61(10) 5_666 .
N2 Mn2 O1 87.56(9) 5_667 .
N2 Mn2 O1 92.44(9) 1_554 .
N1 Mn2 O1 92.61(10) . 5_666
N1 Mn2 O1 87.39(10) 5_666 5_666
N2 Mn2 O1 92.44(9) 5_667 5_666
N2 Mn2 O1 87.56(9) 1_554 5_666
O1 Mn2 O1 180.00(11) . 5_666
N1 C1 Ni1 175.6(3) . .
N2 C2 Ni1 177.9(3) . .
C1 N1 Mn2 158.4(3) . .
C2 N2 Mn2 175.2(3) . 1_556
Mn2 O1 H1A 114.2 . .
Mn2 O1 H1B 108.7 . .
H1A O1 H1B 108.7 . .
Mn2 O1 H1C 108.8 . .
H1A O1 H1C 108.7 . .
H1B O1 H1C 107.6 . .
H2A O2 H2B 107.7 . .
H2A O2 H2C 110.9 . .
H2B O2 H2C 111.9 . .
H3A O3 H3D 119.2 . .
H4A O4 H4B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 C2 1.864(3) 7_565
Ni1 C2 1.864(3) .
Ni1 C1 1.867(3) .
Ni1 C1 1.867(3) 7_565
Mn2 N1 2.197(3) .
Mn2 N1 2.197(3) 5_666
Mn2 N2 2.201(3) 5_667
Mn2 N2 2.201(3) 1_554
Mn2 O1 2.231(2) .
Mn2 O1 2.231(2) 5_666
C1 N1 1.144(4) .
C2 N2 1.147(4) .
N2 Mn2 2.201(3) 1_556
O1 H1A 0.8887 .
O1 H1B 0.8500 .
O1 H1C 0.8500 .
O2 H2A 0.824(14) .
O2 H2B 0.8463 .
O2 H2C 0.8141 .
O3 H3A 0.813(19) .
O3 H3D 0.9110 .
O4 H4A 0.8701 .
O4 H4B 0.8500 .
