#------------------------------------------------------------------------------
#$Date: 2019-11-17 07:48:37 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228739 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/84/1548491.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_1548491
loop_
_publ_author_name
'Craig, Gavin A.'
'Sarkar, Arup'
'Woodall, Christopher H.'
'Hay, Moya A.'
'Marriott, Katie E. R.'
'Kamenev, Konstantin V.'
'Moggach, Stephen A.'
'Brechin, Euan K.'
'Parsons, Simon'
'Rajaraman, Gopalan'
'Murrie, Mark'
_publ_section_title
;
 Probing the origin of the giant magnetic anisotropy in trigonal
 bipyramidal Ni(ii) under high pressure.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1551
_journal_page_last               1559
_journal_paper_doi               10.1039/c7sc04460g
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H30 Cl4 N4 Ni1 O4'
_chemical_formula_sum            'C14 H30 Cl4 N4 Ni O4'
_chemical_formula_weight         518.94
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_audit_update_record
;
2017-10-12 deposited with the CCDC.
2017-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3181(7)
_cell_length_b                   12.8429(7)
_cell_length_c                   13.0380(4)
_cell_measurement_reflns_used    5757
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.50
_cell_volume                     2062.61(17)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_pressure         580
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.483
_diffrn_measured_fraction_theta_max 0.483
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6211
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_min         3.505
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.19
_refine_ls_abs_structure_details 'Flack (1983), 813 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.008(15)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0411
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1710
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.0151733
_refine_ls_shift/su_mean         0.0006231
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 2.17 2.68 0.725 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0706
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0706
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                1588
_reflns_number_total             1738
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0327
_oxford_refine_ls_scale          0.11405(4)
_oxford_reflns_number_all        1710
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7sc04460g2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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.

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

 Adding full bibliography for 1548488--1548492.cif.
;
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_original_formula_sum        'C14 H30 Cl4 N4 Ni1 O4'
_cod_database_code               1548491
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,y,z+1/2
x+1/2,-y,z
-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ni1 Ni 0.45996(7) 0.75171(7) 0.71237(9) 0.0257 1.0000 Uani . .
Cl1 Cl 0.52732(17) 0.60484(16) 0.79045(13) 0.0445 1.0000 Uani . .
Cl3 Cl 0.55700(18) 0.81320(17) 0.57338(12) 0.0487 1.0000 Uani . .
Cl2 Cl 0.30459(18) 0.83627(17) 0.76503(14) 0.0434 1.0000 Uani . .
N11 N 0.3600(5) 0.6502(4) 0.6132(3) 0.0245 1.0000 Uani D U
N12 N 0.2498(5) 0.5218(5) 0.5007(3) 0.0266 1.0000 Uani D U
C11 C 0.2802(6) 0.5906(5) 0.6744(4) 0.0261 1.0000 Uani D U
C12 C 0.2053(6) 0.5266(6) 0.6063(4) 0.0367 1.0000 Uani D U
C13 C 0.2974(7) 0.7050(6) 0.5335(4) 0.0328 1.0000 Uani D U
C14 C 0.2455(8) 0.6303(6) 0.4571(5) 0.0459 1.0000 Uani D U
C15 C 0.4315(6) 0.5751(6) 0.5590(4) 0.0341 1.0000 Uani D U
C16 C 0.3662(7) 0.4896(7) 0.5078(5) 0.0467 1.0000 Uani D U
C17 C 0.1875(7) 0.4483(6) 0.4348(4) 0.0369 1.0000 Uani D U
N21 N 0.5588(5) 0.8471(4) 0.8189(3) 0.0274 1.0000 Uani D U
N22 N 0.6691(5) 0.9558(4) 0.9456(3) 0.0283 1.0000 Uani D U
C21 C 0.5247(6) 0.8257(6) 0.9262(4) 0.0332 1.0000 Uani D U
C22 C 0.6016(7) 0.8785(6) 1.0019(4) 0.0399 1.0000 Uani D U
C23 C 0.5432(6) 0.9593(5) 0.7983(4) 0.0306 1.0000 Uani D U
C24 C 0.5946(6) 1.0233(6) 0.8848(4) 0.0310 1.0000 Uani D U
C25 C 0.6750(6) 0.8214(5) 0.8099(4) 0.0313 1.0000 Uani D U
C26 C 0.7428(6) 0.8987(6) 0.8726(4) 0.0346 1.0000 Uani D U
C27 C 0.7343(8) 1.0173(6) 1.0202(5) 0.0463 1.0000 Uani D U
Cl4 Cl 0.52954(17) 0.72277(16) 1.23016(12) 0.0332 1.0000 Uani . .
O41 O 0.4786(7) 0.7124(6) 1.1343(4) 0.0752 1.0000 Uani . U
O42 O 0.4630(6) 0.6804(6) 1.3081(4) 0.0781 1.0000 Uani . U
O43 O 0.6311(6) 0.6698(5) 1.2265(6) 0.0826 1.0000 Uani . U
O44 O 0.5522(6) 0.8280(5) 1.2497(4) 0.0699 1.0000 Uani . U
H111 H 0.2373 0.6385 0.7133 0.0329 1.0000 Uiso . .
H112 H 0.3173 0.5455 0.7206 0.0329 1.0000 Uiso . .
H121 H 0.1340 0.5561 0.6060 0.0475 1.0000 Uiso . .
H122 H 0.1990 0.4567 0.6343 0.0475 1.0000 Uiso . .
H131 H 0.2413 0.7444 0.5661 0.0407 1.0000 Uiso . .
H132 H 0.3437 0.7497 0.4970 0.0407 1.0000 Uiso . .
H141 H 0.1693 0.6492 0.4474 0.0578 1.0000 Uiso . .
H142 H 0.2803 0.6329 0.3936 0.0578 1.0000 Uiso . .
H151 H 0.4815 0.5454 0.6039 0.0419 1.0000 Uiso . .
H152 H 0.4701 0.6128 0.5058 0.0419 1.0000 Uiso . .
H161 H 0.3722 0.4274 0.5458 0.0610 1.0000 Uiso . .
H162 H 0.3931 0.4773 0.4392 0.0610 1.0000 Uiso . .
H171 H 0.2140 0.4455 0.3681 0.0543 1.0000 Uiso . .
H172 H 0.1112 0.4700 0.4325 0.0543 1.0000 Uiso . .
H173 H 0.1874 0.3795 0.4646 0.0543 1.0000 Uiso . .
H211 H 0.4513 0.8539 0.9375 0.0428 1.0000 Uiso . .
H212 H 0.5199 0.7526 0.9381 0.0428 1.0000 Uiso . .
H221 H 0.5634 0.9096 1.0563 0.0520 1.0000 Uiso . .
H222 H 0.6484 0.8244 1.0308 0.0520 1.0000 Uiso . .
H231 H 0.5732 0.9768 0.7342 0.0350 1.0000 Uiso . .
H232 H 0.4657 0.9739 0.7962 0.0350 1.0000 Uiso . .
H241 H 0.6360 1.0790 0.8550 0.0366 1.0000 Uiso . .
H242 H 0.5405 1.0520 0.9278 0.0366 1.0000 Uiso . .
H251 H 0.6874 0.7536 0.8329 0.0372 1.0000 Uiso . .
H252 H 0.6955 0.8271 0.7388 0.0372 1.0000 Uiso . .
H261 H 0.7980 0.8614 0.9089 0.0408 1.0000 Uiso . .
H262 H 0.7779 0.9475 0.8276 0.0408 1.0000 Uiso . .
H271 H 0.7779 1.0669 0.9864 0.0541 1.0000 Uiso . .
H272 H 0.6883 1.0515 1.0687 0.0541 1.0000 Uiso . .
H273 H 0.7820 0.9713 1.0590 0.0541 1.0000 Uiso . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 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_publ_flag
Cl1 Ni1 Cl3 116.18(9) yes
Cl1 Ni1 Cl2 123.67(8) yes
Cl3 Ni1 Cl2 120.15(9) yes
Cl1 Ni1 N11 88.64(14) yes
Cl3 Ni1 N11 91.77(13) yes
Cl2 Ni1 N11 89.40(16) yes
Cl1 Ni1 N21 88.71(15) yes
Cl3 Ni1 N21 91.07(14) yes
Cl2 Ni1 N21 90.52(16) yes
N11 Ni1 N21 176.76(18) yes
Ni1 N11 C11 111.1(3) yes
Ni1 N11 C13 115.0(4) yes
C11 N11 C13 106.3(5) yes
Ni1 N11 C15 109.3(4) yes
C11 N11 C15 108.3(5) yes
C13 N11 C15 106.6(4) yes
C12 N12 C14 107.4(6) yes
C12 N12 C16 108.0(5) yes
C14 N12 C16 108.3(6) yes
C12 N12 C17 111.8(5) yes
C14 N12 C17 110.5(5) yes
C16 N12 C17 110.8(6) yes
N11 C11 C12 111.6(4) yes
N11 C11 H111 108.7 no
C12 C11 H111 108.8 no
N11 C11 H112 109.8 no
C12 C11 H112 109.4 no
H111 C11 H112 108.6 no
C11 C12 N12 109.8(5) yes
C11 C12 H121 110.2 no
N12 C12 H121 110.7 no
C11 C12 H122 109.1 no
N12 C12 H122 109.8 no
H121 C12 H122 107.1 no
N11 C13 C14 112.3(5) yes
N11 C13 H131 108.5 no
C14 C13 H131 108.7 no
N11 C13 H132 109.3 no
C14 C13 H132 108.0 no
H131 C13 H132 109.9 no
C13 C14 N12 108.7(5) yes
C13 C14 H141 109.3 no
N12 C14 H141 108.2 no
C13 C14 H142 111.4 no
N12 C14 H142 110.6 no
H141 C14 H142 108.5 no
N11 C15 C16 111.4(6) yes
N11 C15 H151 111.0 no
C16 C15 H151 109.3 no
N11 C15 H152 107.9 no
C16 C15 H152 107.9 no
H151 C15 H152 109.3 no
C15 C16 N12 109.6(6) yes
C15 C16 H161 110.0 no
N12 C16 H161 110.0 no
C15 C16 H162 110.1 no
N12 C16 H162 108.4 no
H161 C16 H162 108.7 no
N12 C17 H171 112.5 no
N12 C17 H172 109.3 no
H171 C17 H172 108.6 no
N12 C17 H173 110.5 no
H171 C17 H173 110.0 no
H172 C17 H173 105.7 no
Ni1 N21 C21 109.5(4) yes
Ni1 N21 C23 110.7(4) yes
C21 N21 C23 108.3(5) yes
Ni1 N21 C25 111.1(4) yes
C21 N21 C25 107.9(5) yes
C23 N21 C25 109.2(5) yes
C22 N22 C24 107.8(6) yes
C22 N22 C26 108.9(6) yes
C24 N22 C26 108.5(4) yes
C22 N22 C27 109.5(5) yes
C24 N22 C27 111.8(6) yes
C26 N22 C27 110.3(6) yes
N21 C21 C22 110.6(5) yes
N21 C21 H211 109.4 no
C22 C21 H211 107.9 no
N21 C21 H212 110.7 no
C22 C21 H212 111.7 no
H211 C21 H212 106.3 no
C21 C22 N22 108.9(4) yes
C21 C22 H221 111.5 no
N22 C22 H221 111.7 no
C21 C22 H222 107.4 no
N22 C22 H222 109.5 no
H221 C22 H222 107.8 no
N21 C23 C24 109.6(5) yes
N21 C23 H231 110.2 no
C24 C23 H231 111.3 no
N21 C23 H232 108.7 no
C24 C23 H232 108.8 no
H231 C23 H232 108.3 no
C23 C24 N22 109.5(6) yes
C23 C24 H241 108.7 no
N22 C24 H241 108.7 no
C23 C24 H242 110.8 no
N22 C24 H242 110.2 no
H241 C24 H242 108.8 no
N21 C25 C26 110.0(5) yes
N21 C25 H251 110.0 no
C26 C25 H251 110.1 no
N21 C25 H252 108.3 no
C26 C25 H252 108.7 no
H251 C25 H252 109.7 no
C25 C26 N22 108.9(5) yes
C25 C26 H261 109.0 no
N22 C26 H261 111.1 no
C25 C26 H262 110.0 no
N22 C26 H262 109.9 no
H261 C26 H262 107.9 no
N22 C27 H271 111.2 no
N22 C27 H272 110.9 no
H271 C27 H272 109.6 no
N22 C27 H273 110.0 no
H271 C27 H273 108.0 no
H272 C27 H273 107.0 no
O41 Cl4 O42 110.1(4) yes
O41 Cl4 O43 108.5(5) yes
O42 Cl4 O43 110.4(5) yes
O41 Cl4 O44 110.0(4) yes
O42 Cl4 O44 110.8(4) yes
O43 Cl4 O44 107.0(5) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 Cl1 2.298(2) yes
Ni1 Cl3 2.3101(18) yes
Ni1 Cl2 2.305(2) yes
Ni1 N11 2.212(5) yes
Ni1 N21 2.216(6) yes
N11 C11 1.479(7) yes
N11 C13 1.473(7) yes
N11 C15 1.485(8) yes
N12 C12 1.483(7) yes
N12 C14 1.505(8) yes
N12 C16 1.496(9) yes
N12 C17 1.490(6) yes
C11 C12 1.522(7) yes
C11 H111 0.957 no
C11 H112 0.953 no
C12 H121 0.955 no
C12 H122 0.973 no
C13 C14 1.524(7) yes
C13 H131 0.956 no
C13 H132 0.939 no
C14 H141 0.977 no
C14 H142 0.933 no
C15 C16 1.515(7) yes
C15 H151 0.932 no
C15 H152 0.971 no
C16 H161 0.943 no
C16 H162 0.966 no
C17 H171 0.929 no
C17 H172 0.981 no
C17 H173 0.965 no
N21 C21 1.485(6) yes
N21 C23 1.479(8) yes
N21 C25 1.474(8) yes
N22 C22 1.488(8) yes
N22 C24 1.491(8) yes
N22 C26 1.506(7) yes
N22 C27 1.488(6) yes
C21 C22 1.527(7) yes
C21 H211 0.985 no
C21 H212 0.953 no
C22 H221 0.940 no
C22 H222 0.979 no
C23 C24 1.532(9) yes
C23 H231 0.941 no
C23 H232 0.973 no
C24 H241 0.962 no
C24 H242 0.946 no
C25 C26 1.534(7) yes
C25 H251 0.933 no
C25 H252 0.964 no
C26 H261 0.957 no
C26 H262 0.961 no
C27 H271 0.942 no
C27 H272 0.956 no
C27 H273 0.975 no
Cl4 O41 1.404(5) yes
Cl4 O42 1.415(6) yes
Cl4 O43 1.425(7) yes
Cl4 O44 1.403(6) yes
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
5 1 4 x
6 2 3 x
2 8 4 x
8 3 6 x
9 4 6 x
6 1 7 x
9 4 8 x
3 9 1 x
4 0 5 x
9 4 7 x
8 3 7 x
0 6 14 x
3 9 6 x
3 9 5 x
4 10 -9 x
0 6 -8 x
6 1 14 x
6 1 12 x
1 7 6 x
8 3 8 x
