#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:37:19 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224298 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/93/7049375.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_7049375
loop_
_publ_author_name
'Shen, Lingyi'
'Zhao, Yanxia'
'Luo, Qiong'
'Li, Qian-Shu'
'Liu, Bin'
'Redshaw, Carl'
'Wu, Biao'
'Yang, Xiao-Juan'
_publ_section_title
;
 Cyclotrimerization of alkynes catalyzed by a self-supported cyclic
 tri-nuclear nickel(0) complex with α-diimine ligands.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4643
_journal_page_last               4649
_journal_paper_doi               10.1039/c9dt00819e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C60 H72 Br6 N6 Ni3'
_chemical_formula_weight         1532.82
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-14 deposited with the CCDC.    2019-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.198(5)
_cell_length_b                   13.198(5)
_cell_length_c                   23.606(9)
_cell_measurement_reflns_used    5285
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.48
_cell_volume                     3561(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0969
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16357
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    4.188
_exptl_absorpt_correction_T_max  0.4880
_exptl_absorpt_correction_T_min  0.4208
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_meas      ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         2.154
_refine_diff_density_min         -2.704
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0952
_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)+(0.0080P)²+45.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1313
_reflns_number_total             2136
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00819e2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7049375--7049377.cif.
;
_cod_original_cell_volume        3561(3)
_cod_database_code               7049375
_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   0.421
_shelx_estimated_absorpt_t_max   0.488
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -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 0.52241(15) 0.21397(16) 0.2500 0.0416(5) Uani 1 2 d S T P
Br1 Br 0.6667 0.3333 0.17251(17) 0.1244(13) Uani 1 3 d S T P
Br2 Br 0.62682(14) 0.08944(14) 0.2500 0.0565(5) Uani 1 2 d S T P
Br3 Br 0.0000 0.0000 0.2500 0.1062(14) Uani 1 6 d S T P
N1 N 0.3953(7) 0.1012(7) 0.1945(4) 0.051(2) Uani 1 1 d . . .
C1 C 0.3079(9) 0.0151(9) 0.2182(5) 0.052(3) Uani 1 1 d . . .
C2 C 0.2093(11) -0.0831(11) 0.1883(6) 0.086(4) Uani 1 1 d . . .
H2A H 0.1384 -0.0821 0.1962 0.129 Uiso 1 1 calc R U .
H2B H 0.2014 -0.1557 0.2011 0.129 Uiso 1 1 calc R U .
H2C H 0.2239 -0.0752 0.1483 0.129 Uiso 1 1 calc R U .
C3 C 0.4045(10) 0.1173(11) 0.1339(5) 0.059(3) Uani 1 1 d . . .
C4 C 0.4829(14) 0.0921(15) 0.1072(5) 0.099(5) Uani 1 1 d . . .
H4 H 0.5215 0.0595 0.1262 0.119 Uiso 1 1 calc R U .
C5 C 0.5004(17) 0.1203(16) 0.0466(6) 0.110(6) Uani 1 1 d . . .
H5 H 0.5573 0.1116 0.0276 0.132 Uiso 1 1 calc R U .
C6 C 0.4409(15) 0.1569(16) 0.0181(6) 0.099(5) Uani 1 1 d . . .
C7 C 0.3627(14) 0.1789(14) 0.0465(7) 0.097(5) Uani 1 1 d . . .
H7 H 0.3217 0.2070 0.0260 0.117 Uiso 1 1 calc R U .
C8 C 0.3415(12) 0.1598(12) 0.1072(6) 0.074(4) Uani 1 1 d . . .
C9 C 0.2561(16) 0.1814(16) 0.1331(7) 0.112(6) Uani 1 1 d . . .
H9A H 0.2005 0.1129 0.1534 0.168 Uiso 1 1 calc R U .
H9B H 0.2163 0.1998 0.1044 0.168 Uiso 1 1 calc R U .
H9C H 0.2942 0.2459 0.1590 0.168 Uiso 1 1 calc R U .
C10 C 0.4600(18) 0.1850(18) -0.0445(6) 0.150(9) Uani 1 1 d . . .
H10A H 0.5147 0.2668 -0.0494 0.226 Uiso 1 1 calc R U .
H10B H 0.3869 0.1661 -0.0619 0.226 Uiso 1 1 calc R U .
H10C H 0.4903 0.1398 -0.0617 0.226 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'
Br Br -0.2901 2.4595 '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'
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
N1 Ni1 N1 79.0(5) 10_556 .
N1 Ni1 Br1 173.0(3) 10_556 .
N1 Ni1 Br1 94.4(3) . .
N1 Ni1 Br1 94.4(3) 10_556 8_666
N1 Ni1 Br1 173.0(3) . 8_666
Br1 Ni1 Br1 92.12(14) . 8_666
N1 Ni1 Br2 96.8(2) 10_556 8_666
N1 Ni1 Br2 96.8(2) . 8_666
Br1 Ni1 Br2 86.26(6) . 8_666
Br1 Ni1 Br2 86.26(6) 8_666 8_666
N1 Ni1 Br2 92.3(2) 10_556 .
N1 Ni1 Br2 92.3(2) . .
Br1 Ni1 Br2 85.57(5) . .
Br1 Ni1 Br2 85.57(5) 8_666 .
Br2 Ni1 Br2 168.22(8) 8_666 .
Ni1 Br1 Ni1 73.87(11) 3_655 .
Ni1 Br1 Ni1 73.87(11) 3_655 8_666
Ni1 Br1 Ni1 73.87(11) . 8_666
Ni1 Br2 Ni1 71.78(8) 3_655 .
C1 N1 C3 122.6(9) . .
C1 N1 Ni1 114.3(7) . .
C3 N1 Ni1 123.1(7) . .
N1 C1 C2 125.5(10) . .
N1 C1 C1 116.0(6) . 10_556
C2 C1 C1 118.5(7) . 10_556
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C8 C3 C4 124.6(11) . .
C8 C3 N1 119.6(11) . .
C4 C3 N1 115.8(11) . .
C3 C4 C5 115.2(14) . .
C3 C4 H4 122.4 . .
C5 C4 H4 122.4 . .
C6 C5 C4 123.5(16) . .
C6 C5 H5 118.2 . .
C4 C5 H5 118.2 . .
C5 C6 C7 118.9(15) . .
C5 C6 C10 122.7(18) . .
C7 C6 C10 118.3(18) . .
C6 C7 C8 122.7(15) . .
C6 C7 H7 118.6 . .
C8 C7 H7 118.6 . .
C3 C8 C9 125.8(13) . .
C3 C8 C7 114.9(13) . .
C9 C8 C7 119.3(14) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C6 C10 H10A 109.5 . .
C6 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C6 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.062(8) 10_556
Ni1 N1 2.062(8) .
Ni1 Br1 2.540(3) .
Ni1 Br1 2.540(3) 8_666
Ni1 Br2 2.588(3) 8_666
Ni1 Br2 2.620(3) .
Br1 Ni1 2.540(3) 3_655
Br1 Ni1 2.540(3) 8_666
Br2 Ni1 2.588(3) 3_655
N1 C1 1.275(13) .
N1 C3 1.441(13) .
C1 C2 1.477(14) .
C1 C1 1.50(2) 10_556
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C8 1.369(16) .
C3 C4 1.387(17) .
C4 C5 1.47(2) .
C4 H4 0.9300 .
C5 C6 1.30(2) .
C5 H5 0.9300 .
C6 C7 1.38(2) .
C6 C10 1.51(2) .
C7 C8 1.458(19) .
C7 H7 0.9300 .
C8 C9 1.431(19) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
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_4
C3 N1 C1 C2 4.3(18) .
Ni1 N1 C1 C2 -175.1(10) .
C3 N1 C1 C1 -176.2(8) 10_556
Ni1 N1 C1 C1 4.4(8) 10_556
C1 N1 C3 C8 77.2(15) .
Ni1 N1 C3 C8 -103.5(12) .
C1 N1 C3 C4 -105.5(14) .
Ni1 N1 C3 C4 73.9(14) .
C8 C3 C4 C5 3(2) .
N1 C3 C4 C5 -173.9(13) .
C3 C4 C5 C6 -6(3) .
C4 C5 C6 C7 5(3) .
C4 C5 C6 C10 -179.6(16) .
C5 C6 C7 C8 -2(3) .
C10 C6 C7 C8 -177.3(14) .
C4 C3 C8 C9 176.9(15) .
N1 C3 C8 C9 -6(2) .
C4 C3 C8 C7 0(2) .
N1 C3 C8 C7 176.6(11) .
C6 C7 C8 C3 -1(2) .
C6 C7 C8 C9 -178.1(16) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 120 37 ' '
2 0.000 0.000 0.500 120 37 ' '
3 0.333 0.667 0.250 209 58 ' '
4 0.667 0.333 0.750 209 58 ' '
