#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:12:25 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223957 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048711.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_7048711
loop_
_publ_author_name
'Chakraborty, Tonmoy'
'Mukherjee, Somali'
'Dasgupta, Sanchari'
'Biswas, Biplab'
'Das, Debasis'
_publ_section_title
;
 Anion-mediated bio-relevant catalytic activity of dinuclear nickel(ii)
 complexes derived from an end-off compartmental ligand.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2772
_journal_page_last               2784
_journal_paper_doi               10.1039/c8dt04631j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C27 H35 Cl3 N4 Ni2 O3'
_chemical_formula_sum            'C27 H35 Cl3 N4 Ni2 O3'
_chemical_formula_weight         687.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-06 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.391(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6797(16)
_cell_length_b                   12.8141(16)
_cell_length_c                   14.3303(15)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.918
_cell_measurement_theta_min      2.031
_cell_volume                     2956.8(6)
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2016/1 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20628
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.918
_diffrn_reflns_theta_min         2.031
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1150 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.6825.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1424.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.777
_exptl_transmission_factor_min   0.641
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3180
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0588P)²+1.9245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2759
_reflns_number_total             3201
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04631j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7048710--7048712.cif.'
_cod_database_code               7048711
_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_max   0.777
_shelx_estimated_absorpt_t_min   0.641
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.01
 Ni1-H2
 2.794912 with sigma of 0.02
 C1-H2
 1.898485 with sigma of 0.02
3. Others
 Fixed Sof: C15A(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C15B(0.5) H15D(0.5)
 H15E(0.5) H15F(0.5) C14(0.5) H14(0.5)
4.a Ternary CH refined with riding coordinates:
 C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
4.c Me refined with riding coordinates:
 C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C9(H9), C12(H12)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.94668(2) 0.27292(2) 0.32100(2) 0.03325(12) Uani 1 1 d D . . . .
Cl1 Cl 1.06942(4) 0.27565(5) 0.47653(5) 0.04722(17) Uani 1 1 d . . . . .
Cl2 Cl 1.000000 0.13861(5) 0.250000 0.03597(18) Uani 1 2 d S T P . .
O1 O 1.000000 0.37102(15) 0.250000 0.0364(5) Uani 1 2 d S T P . .
O2 O 0.84192(11) 0.27318(13) 0.17147(14) 0.0480(4) Uani 1 1 d D . . . .
H2 H 0.8553(13) 0.2898(19) 0.1211(11) 0.072 Uiso 1 1 d DR . . . .
N1 N 0.88202(12) 0.16572(16) 0.37445(14) 0.0423(4) Uani 1 1 d . . . . .
N2 N 0.90120(14) 0.39488(16) 0.36725(16) 0.0476(5) Uani 1 1 d . . . . .
C1 C 0.79176(18) 0.1819(3) 0.1311(2) 0.0682(8) Uani 1 1 d D . . . .
H1A H 0.749176 0.178683 0.156181 0.102 Uiso 1 1 calc GR . . . .
H1B H 0.825975 0.120736 0.152457 0.102 Uiso 1 1 calc GR . . . .
H1C H 0.766610 0.185405 0.057604 0.102 Uiso 1 1 calc GR . . . .
C2 C 0.90889(17) 0.06697(19) 0.39257(19) 0.0502(6) Uani 1 1 d . . . . .
H2A H 0.961423 0.052038 0.395894 0.060 Uiso 1 1 calc R . . . .
C3 C 0.8636(2) -0.0130(2) 0.4064(2) 0.0658(8) Uani 1 1 d . . . . .
H3 H 0.885071 -0.080368 0.419168 0.079 Uiso 1 1 calc R . . . .
C4 C 0.7861(2) 0.0077(3) 0.4013(3) 0.0762(9) Uani 1 1 d . . . . .
H4 H 0.752600 -0.045586 0.407107 0.091 Uiso 1 1 calc R . . . .
C5 C 0.75905(18) 0.1097(3) 0.3872(2) 0.0687(8) Uani 1 1 d . . . . .
H5 H 0.707317 0.126086 0.385661 0.082 Uiso 1 1 calc R . . . .
C6 C 0.80781(16) 0.1871(2) 0.3753(2) 0.0528(6) Uani 1 1 d . . . . .
C7 C 0.7817(2) 0.2995(3) 0.3664(3) 0.0730(9) Uani 1 1 d . . . . .
H7A H 0.758024 0.319162 0.294596 0.088 Uiso 1 1 calc R . . . .
H7B H 0.738565 0.306884 0.391202 0.088 Uiso 1 1 calc R . . . .
C8 C 0.8512(2) 0.3732(2) 0.4246(3) 0.0680(8) Uani 1 1 d . . . . .
H8A H 0.828427 0.437949 0.437012 0.082 Uiso 1 1 calc R . . . .
H8B H 0.886054 0.342819 0.490405 0.082 Uiso 1 1 calc R . . . .
C9 C 0.91463(18) 0.4897(2) 0.3551(2) 0.0525(6) Uani 1 1 d . . . . .
H9 H 0.892104 0.538151 0.384751 0.063 Uiso 1 1 calc R . . . .
C11 C 1.03946(17) 0.53205(17) 0.19919(18) 0.0467(6) Uani 1 1 d . . . . .
C12 C 1.0384(2) 0.64095(19) 0.20083(19) 0.0612(8) Uani 1 1 d . . . . .
H12 H 1.065063 0.677101 0.166815 0.073 Uiso 1 1 calc R . . . .
C13 C 1.000000 0.6970(3) 0.250000 0.0692(13) Uani 1 2 d S T P . .
C10 C 1.000000 0.4732(2) 0.250000 0.0374(6) Uani 1 2 d S T P . .
C15A C 0.9502(9) 0.8621(10) 0.1453(9) 0.059(2) Uani 0.5 1 d . . . A -1
H15A H 0.897580 0.831680 0.102582 0.088 Uiso 0.5 1 calc R . . A -1
H15B H 0.943933 0.936169 0.149110 0.088 Uiso 0.5 1 calc R . . A -1
H15C H 0.989609 0.847797 0.116804 0.088 Uiso 0.5 1 calc R . . A -1
C15B C 1.0633(8) 0.8614(8) 0.3212(8) 0.071(3) Uani 0.5 1 d . . . A -1
H15D H 1.081193 0.830656 0.387948 0.106 Uiso 0.5 1 calc R . . A -1
H15E H 1.103564 0.847164 0.293905 0.106 Uiso 0.5 1 calc R . . A -1
H15F H 1.057888 0.935536 0.326212 0.106 Uiso 0.5 1 calc R . . A -1
C14 C 0.9807(3) 0.8159(3) 0.2512(6) 0.0424(13) Uani 0.5 1 d . . . A -1
H14 H 0.939724 0.826885 0.279949 0.051 Uiso 0.5 1 calc R . . A -1
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'
Cl Cl 0.1484 0.1585 '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
Cl2 Ni1 Cl1 92.402(17) . .
O1 Ni1 Cl1 91.554(19) . .
O1 Ni1 Cl2 83.58(4) . .
O1 Ni1 O2 83.72(5) . .
O1 Ni1 N1 172.62(6) . .
O2 Ni1 Cl1 174.67(5) . .
O2 Ni1 Cl2 84.64(5) . .
N1 Ni1 Cl1 95.17(5) . .
N1 Ni1 Cl2 93.07(6) . .
N1 Ni1 O2 89.43(7) . .
N2 Ni1 Cl1 90.80(7) . .
N2 Ni1 Cl2 173.67(6) . .
N2 Ni1 O1 90.88(7) . .
N2 Ni1 O2 91.72(8) . .
N2 Ni1 N1 92.07(8) . .
Ni1 Cl2 Ni1 87.51(3) 2_755 .
Ni1 O1 Ni1 105.33(9) . 2_755
C10 O1 Ni1 127.33(4) . .
C10 O1 Ni1 127.33(4) . 2_755
Ni1 O2 H2 113.7(13) . .
C1 O2 Ni1 121.85(16) . .
C1 O2 H2 101.4(13) . .
C2 N1 Ni1 118.74(16) . .
C2 N1 C6 117.4(2) . .
C6 N1 Ni1 122.98(17) . .
C8 N2 Ni1 117.34(17) . .
C9 N2 Ni1 125.71(18) . .
C9 N2 C8 116.9(2) . .
O2 C1 H1A 109.5 . .
O2 C1 H1B 109.5 . .
O2 C1 H1C 109.5 . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 118.1 . .
N1 C2 C3 123.7(3) . .
C3 C2 H2A 118.1 . .
C2 C3 H3 120.6 . .
C2 C3 C4 118.8(3) . .
C4 C3 H3 120.6 . .
C3 C4 H4 120.9 . .
C3 C4 C5 118.1(3) . .
C5 C4 H4 120.9 . .
C4 C5 H5 119.8 . .
C6 C5 C4 120.5(3) . .
C6 C5 H5 119.8 . .
N1 C6 C5 121.3(3) . .
N1 C6 C7 117.4(2) . .
C5 C6 C7 121.2(3) . .
C6 C7 H7A 108.8 . .
C6 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
C8 C7 C6 113.8(3) . .
C8 C7 H7A 108.8 . .
C8 C7 H7B 108.8 . .
N2 C8 C7 110.7(3) . .
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
N2 C9 H9 116.0 . .
N2 C9 C11 128.0(2) . 2_755
C11 C9 H9 116.0 2_755 .
C12 C11 C9 113.6(2) . 2_755
C12 C11 C10 120.7(2) . .
C10 C11 C9 125.7(2) . 2_755
C11 C12 H12 118.4 . .
C13 C12 C11 123.2(3) . .
C13 C12 H12 118.4 . .
C12 C13 C12 116.6(3) . 2_755
C12 C13 C14 132.5(3) . .
C12 C13 C14 110.5(2) 2_755 .
O1 C10 C11 122.17(14) . .
O1 C10 C11 122.17(14) . 2_755
C11 C10 C11 115.7(3) . 2_755
H15A C15A H15B 109.5 . .
H15A C15A H15C 109.5 . .
H15B C15A H15C 109.5 . .
C14 C15A H15A 109.5 . .
C14 C15A H15B 109.5 . .
C14 C15A H15C 109.5 . .
H15D C15B H15E 109.5 . .
H15D C15B H15F 109.5 . .
H15E C15B H15F 109.5 . .
C14 C15B H15D 109.5 . .
C14 C15B H15E 109.5 . .
C14 C15B H15F 109.5 . .
C13 C14 H14 110.3 . .
C15A C14 C13 111.1(6) . .
C15A C14 C15B 111.3(6) . .
C15A C14 H14 110.3 . .
C15B C14 C13 103.2(5) . .
C15B C14 H14 110.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 Cl1 2.3840(7) .
Ni1 Cl2 2.3830(6) .
Ni1 O1 2.0727(12) .
Ni1 O2 2.1781(18) .
Ni1 N1 2.1223(19) .
Ni1 N2 1.9920(19) .
O1 C10 1.310(3) .
O2 H2 0.874(9) .
O2 C1 1.437(4) .
N1 C2 1.339(3) .
N1 C6 1.345(3) .
N2 C8 1.461(3) .
N2 C9 1.264(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9300 .
C2 C3 1.365(4) .
C3 H3 0.9300 .
C3 C4 1.367(5) .
C4 H4 0.9300 .
C4 C5 1.378(5) .
C5 H5 0.9300 .
C5 C6 1.370(4) .
C6 C7 1.502(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.500(5) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9 0.9300 .
C9 C11 1.442(4) 2_755
C11 C12 1.396(3) .
C11 C10 1.416(3) .
C12 H12 0.9300 .
C12 C13 1.367(4) .
C13 C14 1.563(5) .
C15A H15A 0.9600 .
C15A H15B 0.9600 .
C15A H15C 0.9600 .
C15A C14 1.506(13) .
C15B H15D 0.9600 .
C15B H15E 0.9600 .
C15B H15F 0.9600 .
C15B C14 1.506(14) .
C14 H14 0.9800 .
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
O2 H2 Cl1 0.874(9) 2.302(16) 3.1149(19) 155(2) 2_755 yes
C1 H1B Cl2 0.96 2.81 3.404(3) 120.5 . yes
C2 H2A Cl2 0.93 2.69 3.214(2) 116.3 . yes
C3 H3 Cl1 0.93 2.85 3.728(3) 156.9 5_756 yes
