#------------------------------------------------------------------------------
#$Date: 2019-04-19 02:44:19 +0300 (Fri, 19 Apr 2019) $
#$Revision: 214697 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/26/7232639.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_7232639
loop_
_publ_author_name
'Angamuthu, Raja'
'Raje, Sakthi'
_publ_section_title
;
 Solvent-Free Synthesis and Reactivity of Nickel(II) Borohydride and
 Nickel(II) Hydride
;
_journal_name_full               'Green Chemistry'
_journal_paper_doi               10.1039/C8GC04058C
_journal_year                    2019
_chemical_formula_moiety         'C28 H32 Br4 N8 Ni2'
_chemical_formula_sum            'C28 H32 Br4 N8 Ni2'
_chemical_formula_weight         917.67
_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'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.240(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.109(3)
_cell_length_b                   15.035(3)
_cell_length_c                   10.6611(19)
_cell_measurement_reflns_used    5409
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.71
_cell_volume                     2172.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2825
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.392
_diffrn_reflns_theta_min         2.709
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0966P)²+6.7611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2079
_reflns_number_total             2825
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8gc04058c2.cif
_cod_data_source_block           '[(LH)Ni(mu-Br)2Ni(LH)]Br2'
_cod_database_code               7232639
_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.
;
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
Ni Ni 0.38834(6) 0.5000 0.52569(9) 0.0178(2) Uani 1 2 d S T P
Br1 Br 0.5000 0.61628(4) 0.5000 0.0254(2) Uani 1 2 d S T P
Br2 Br 0.30271(7) 0.5000 0.02804(9) 0.0565(4) Uani 1 2 d S T P
N1 N 0.4507(4) 0.5000 0.7491(6) 0.0222(12) Uani 1 2 d S T P
H1C H 0.5243 0.5000 0.7877 0.027 Uiso 1 2 calc R U P
N2 N 0.3022(3) 0.4084(3) 0.5523(4) 0.0183(8) Uani 1 1 d . . .
N3 N 0.2665(4) 0.5000 0.3194(6) 0.0226(12) Uani 1 2 d S T P
H3B H 0.2933 0.5000 0.2488 0.027 Uiso 1 2 calc R U P
C1 C 0.4194(4) 0.4170(3) 0.7931(5) 0.0231(10) Uani 1 1 d . . .
H1A H 0.4144 0.4278 0.8814 0.028 Uiso 1 1 calc R U .
H1B H 0.4699 0.3704 0.8112 0.028 Uiso 1 1 calc R U .
C2 C 0.3209(4) 0.3844(3) 0.6828(5) 0.0221(10) Uani 1 1 d . . .
C3 C 0.2551(4) 0.3334(3) 0.7081(6) 0.0277(11) Uani 1 1 d . . .
H3A H 0.2682 0.3173 0.8008 0.033 Uiso 1 1 calc R U .
C4 C 0.1692(4) 0.3060(3) 0.5955(6) 0.0301(12) Uani 1 1 d . . .
H4A H 0.1234 0.2699 0.6110 0.036 Uiso 1 1 calc R U .
C5 C 0.1493(4) 0.3308(3) 0.4606(6) 0.0295(12) Uani 1 1 d . . .
H5A H 0.0907 0.3120 0.3828 0.035 Uiso 1 1 calc R U .
C6 C 0.2183(4) 0.3842(3) 0.4425(5) 0.0232(10) Uani 1 1 d . . .
C7 C 0.2091(4) 0.4173(3) 0.3028(6) 0.0285(11) Uani 1 1 d . . .
H7A H 0.2332 0.3709 0.2596 0.034 Uiso 1 1 calc R U .
H7B H 0.1388 0.4287 0.2394 0.034 Uiso 1 1 calc R U .
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'
Br Br -0.2901 2.4595 '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
N2 Ni N2 87.1(2) 6_565 .
N2 Ni N1 80.55(16) 6_565 .
N2 Ni N1 80.55(16) . .
N2 Ni N3 80.17(16) 6_565 .
N2 Ni N3 80.16(16) . .
N1 Ni N3 153.3(2) . .
N2 Ni Br1 178.26(12) 6_565 5_666
N2 Ni Br1 92.66(11) . 5_666
N1 Ni Br1 97.71(11) . 5_666
N3 Ni Br1 101.49(11) . 5_666
N2 Ni Br1 92.66(11) 6_565 .
N2 Ni Br1 178.26(12) . .
N1 Ni Br1 97.71(11) . .
N3 Ni Br1 101.49(11) . .
Br1 Ni Br1 87.55(4) 5_666 .
Ni Br1 Ni 92.45(4) . 5_666
C1 N1 C1 114.7(5) . 6_565
C1 N1 Ni 107.9(3) . .
C1 N1 Ni 107.9(3) 6_565 .
C1 N1 H1C 108.7 . .
C1 N1 H1C 108.7 6_565 .
Ni N1 H1C 108.7 . .
C2 N2 C6 121.1(4) . .
C2 N2 Ni 118.7(3) . .
C6 N2 Ni 119.1(3) . .
C7 N3 C7 114.2(6) . 6_565
C7 N3 Ni 108.2(3) . .
C7 N3 Ni 108.2(3) 6_565 .
C7 N3 H3B 108.7 . .
C7 N3 H3B 108.7 6_565 .
Ni N3 H3B 108.7 . .
N1 C1 C2 111.6(4) . .
N1 C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 108.0 . .
N2 C2 C3 121.0(5) . .
N2 C2 C1 113.8(4) . .
C3 C2 C1 125.2(5) . .
C2 C3 C4 118.6(5) . .
C2 C3 H3A 120.7 . .
C4 C3 H3A 120.7 . .
C3 C4 C5 120.6(5) . .
C3 C4 H4A 119.7 . .
C5 C4 H4A 119.7 . .
C4 C5 C6 117.8(5) . .
C4 C5 H5A 121.1 . .
C6 C5 H5A 121.1 . .
N2 C6 C5 120.8(5) . .
N2 C6 C7 114.1(4) . .
C5 C6 C7 125.1(5) . .
N3 C7 C6 111.4(4) . .
N3 C7 H7A 109.4 . .
C6 C7 H7A 109.4 . .
N3 C7 H7B 109.4 . .
C6 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N2 2.000(4) 6_565
Ni N2 2.000(4) .
Ni N1 2.139(6) .
Ni N3 2.156(6) .
Ni Br1 2.5269(8) 5_666
Ni Br1 2.5270(8) .
Br1 Ni 2.5270(8) 5_666
N1 C1 1.483(5) .
N1 C1 1.483(5) 6_565
N1 H1C 1.0000 .
N2 C2 1.340(6) .
N2 C6 1.341(6) .
N3 C7 1.481(6) .
N3 C7 1.481(6) 6_565
N3 H3B 1.0000 .
C1 C2 1.513(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.373(7) .
C3 C4 1.385(7) .
C3 H3A 0.9500 .
C4 C5 1.385(8) .
C4 H4A 0.9500 .
C5 C6 1.394(7) .
C5 H5A 0.9500 .
C6 C7 1.518(7) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
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
N1 H1C Br2 1.00 2.48 3.420(6) 156.5 5_666
N3 H3B Br2 1.00 2.42 3.383(6) 161.7 .
C1 H1A Br2 0.99 2.97 3.852(5) 149.4 1_556
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
C1 N1 C1 C2 91.6(6) 6_565
Ni N1 C1 C2 -28.7(5) .
C6 N2 C2 C3 0.7(7) .
Ni N2 C2 C3 169.0(4) .
C6 N2 C2 C1 179.5(4) .
Ni N2 C2 C1 -12.2(5) .
N1 C1 C2 N2 27.8(6) .
N1 C1 C2 C3 -153.5(5) .
N2 C2 C3 C4 0.9(7) .
C1 C2 C3 C4 -177.8(5) .
C2 C3 C4 C5 -1.0(8) .
C3 C4 C5 C6 -0.3(8) .
C2 N2 C6 C5 -2.1(7) .
Ni N2 C6 C5 -170.4(4) .
C2 N2 C6 C7 179.8(4) .
Ni N2 C6 C7 11.5(5) .
C4 C5 C6 N2 1.9(7) .
C4 C5 C6 C7 179.8(5) .
C7 N3 C7 C6 -92.6(6) 6_565
Ni N3 C7 C6 28.0(5) .
N2 C6 C7 N3 -26.9(6) .
C5 C6 C7 N3 155.1(5) .
