#------------------------------------------------------------------------------
#$Date: 2019-11-23 03:21:51 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231993 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/68/4346806.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_4346806
loop_
_publ_author_name
'Stevens, Charlotte J.'
'Prescimone, Alessandro'
'Tuna, Floriana'
'McInnes, Eric J. L.'
'Parsons, Simon'
'Morrison, Carole A.'
'Arnold, Polly L.'
'Love, Jason B.'
_publ_section_title
;
 Inter- versus Intramolecular Structural Manipulation of a Dichromium(II)
 Pacman Complex through Pressure Variation.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              214
_journal_page_last               220
_journal_paper_doi               10.1021/acs.inorgchem.5b02151
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        C.Stevens
_chemical_formula_moiety         'C48 H46 Cr2 N8'
_chemical_formula_sum            'C48 H46 Cr2 N8'
_chemical_formula_weight         838.94
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'from 1.6 GPa structure'
_audit_creation_date             2014-08-21
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 117.283(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4480(15)
_cell_length_b                   13.1780(12)
_cell_length_c                   14.8896(13)
_cell_measurement_reflns_used    41852
_cell_measurement_temperature    3000
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_volume                     3565.9(5)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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         2100000
_diffrn_ambient_temperature      3000
_diffrn_measured_fraction_theta_full 0.620
_diffrn_measured_fraction_theta_max 0.620
_diffrn_measurement_device       'Rigaku Saturn 724 CCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type
'Synchrotron - Diamond Light Source Beamline I19'
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7647
_diffrn_reflns_theta_full        17.689
_diffrn_reflns_theta_max         17.689
_diffrn_reflns_theta_min         2.300
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method
; 
 
;
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         1852
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.0003938
_refine_ls_shift/su_mean         0.0000588
_refine_ls_structure_factor_coef F
_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: 
 0.196 -0.289 -0.120 -0.251 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0308
_refine_ls_wR_factor_gt          0.0241
_refine_ls_wR_factor_ref         0.0241
_reflns_limit_h_max              22
_reflns_limit_h_min              -25
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1852
_reflns_number_total             2265
_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   0.0530
_oxford_refine_ls_scale          0.1645(5)
_oxford_reflns_number_all        2244
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'crpak4_0m in C2/c'
_cod_data_source_file            2_10GPa.cif
_cod_data_source_block           2_10GPa
_cod_original_cell_volume        3565.9(3)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4346806
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cr1 Cr 0.58427(2) 0.66525(3) 0.77802(3) 0.0232 1.0000 Uani . U
N1 N 0.54176(11) 0.73191(17) 0.86851(17) 0.0225 1.0000 Uani . U
N2 N 0.58548(11) 0.54739(17) 0.85954(16) 0.0213 1.0000 Uani . U
N3 N 0.64916(10) 0.58441(16) 0.74123(16) 0.0202 1.0000 Uani . U
N4 N 0.60313(10) 0.76519(16) 0.68561(16) 0.0220 1.0000 Uani . U
C1 C 0.53994(12) 0.6651(2) 0.93461(19) 0.0214 1.0000 Uani . U
C2 C 0.56545(12) 0.5656(2) 0.93403(19) 0.0214 1.0000 Uani . U
C3 C 0.58227(14) 0.4809(2) 0.99770(19) 0.0253 1.0000 Uani . U
C4 C 0.61359(14) 0.4107(2) 0.9576(2) 0.0266 1.0000 Uani . U
C5 C 0.61634(12) 0.4556(2) 0.87418(19) 0.0203 1.0000 Uani . U
C6 C 0.64255(13) 0.41101(19) 0.80229(19) 0.0220 1.0000 Uani . U
C7 C 0.69460(14) 0.3238(2) 0.8517(2) 0.0324 1.0000 Uani . U
C8 C 0.57397(14) 0.3729(2) 0.7091(2) 0.0273 1.0000 Uani . U
C9 C 0.67812(12) 0.49130(19) 0.76412(18) 0.0198 1.0000 Uani . U
C10 C 0.73390(13) 0.4828(2) 0.7354(2) 0.0250 1.0000 Uani . U
C11 C 0.73991(13) 0.5754(2) 0.6951(2) 0.0259 1.0000 Uani . U
C12 C 0.68605(12) 0.6392(2) 0.69922(19) 0.0218 1.0000 Uani . U
C13 C 0.65524(12) 0.73618(19) 0.66361(18) 0.0202 1.0000 Uani . U
C14 C 0.55617(12) 0.84930(19) 0.64925(18) 0.0195 1.0000 Uani . U
C15 C 0.57825(13) 0.9476(2) 0.6415(2) 0.0241 1.0000 Uani . U
C16 C 0.53068(15) 1.0295(2) 0.62446(19) 0.0263 1.0000 Uani . U
C17 C 0.5597(2) 1.1328(2) 0.6214(2) 0.0384 1.0000 Uani . U
C18 C 0.5916(2) 1.0991(3) 0.8997(3) 0.0468 1.0000 Uani . U
C19 C 0.53936(14) 1.0129(2) 0.8854(2) 0.0284 1.0000 Uani . U
C20 C 0.56279(13) 0.9142(2) 0.8821(2) 0.0254 1.0000 Uani . U
C21 C 0.51633(13) 0.83235(19) 0.86871(18) 0.0202 1.0000 Uani . U
C22 C 0.77801(17) 0.7690(3) 0.9333(3) 0.0445 1.0000 Uani . U
C23 C 0.76541(16) 0.6698(3) 0.9533(3) 0.0441 1.0000 Uani . U
C24 C 0.73764(17) 0.6518(3) 1.0203(3) 0.0449 1.0000 Uani . U
H11 H 0.5219 0.6840 0.9807 0.0256 1.0000 Uiso R .
H31 H 0.5742 0.4727 1.0552 0.0299 1.0000 Uiso R .
H41 H 0.6301 0.3444 0.9829 0.0319 1.0000 Uiso R .
H71 H 0.7106 0.2967 0.8060 0.0385 1.0000 Uiso R .
H72 H 0.7360 0.3471 0.9108 0.0385 1.0000 Uiso R .
H73 H 0.6699 0.2725 0.8694 0.0385 1.0000 Uiso R .
H81 H 0.5882 0.3443 0.6621 0.0327 1.0000 Uiso R .
H82 H 0.5414 0.4281 0.6784 0.0327 1.0000 Uiso R .
H83 H 0.5499 0.3228 0.7292 0.0327 1.0000 Uiso R .
H101 H 0.7627 0.4240 0.7422 0.0302 1.0000 Uiso R .
H111 H 0.7736 0.5922 0.6698 0.0308 1.0000 Uiso R .
H131 H 0.6716 0.7779 0.6258 0.0247 1.0000 Uiso R .
H151 H 0.6261 0.9589 0.6478 0.0293 1.0000 Uiso R .
H171 H 0.5225 1.1819 0.6095 0.0462 1.0000 Uiso R .
H172 H 0.6013 1.1466 0.6842 0.0462 1.0000 Uiso R .
H173 H 0.5735 1.1356 0.5687 0.0462 1.0000 Uiso R .
H181 H 0.6365 1.0728 0.9051 0.0567 1.0000 Uiso R .
H182 H 0.6009 1.1352 0.9596 0.0567 1.0000 Uiso R .
H183 H 0.5703 1.1435 0.8434 0.0567 1.0000 Uiso R .
H201 H 0.6108 0.9029 0.8890 0.0301 1.0000 Uiso R .
H221 H 0.7974 0.7817 0.8873 0.0537 1.0000 Uiso R .
H231 H 0.7759 0.6146 0.9209 0.0537 1.0000 Uiso R .
H241 H 0.7294 0.5841 1.0344 0.0541 1.0000 Uiso R .
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 0.0006 0.0007 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 0.0016 0.0014 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'
Cr 0.2102 0.3048 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399
1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 5_656 Cr1 N1 . 81.80(9) yes
N1 5_656 Cr1 N2 . 120.20(8) yes
N1 . Cr1 N2 . 79.99(9) yes
N1 5_656 Cr1 N3 . 118.45(8) yes
N1 . Cr1 N3 . 159.37(9) yes
N2 . Cr1 N3 . 85.68(9) yes
N1 5_656 Cr1 N4 . 69.39(7) yes
N1 . Cr1 N4 . 114.78(9) yes
N2 . Cr1 N4 . 164.33(9) yes
N3 . Cr1 N4 . 78.69(9) yes
Cr1 . N1 Cr1 5_656 82.27(7) yes
Cr1 . N1 C1 . 110.92(17) yes
Cr1 5_656 N1 C1 . 92.48(15) yes
Cr1 . N1 C21 . 130.49(17) yes
Cr1 5_656 N1 C21 . 95.26(13) yes
C1 . N1 C21 . 118.6(2) yes
Cr1 . N2 C2 . 116.01(17) yes
Cr1 . N2 C5 . 133.51(19) yes
C2 . N2 C5 . 108.7(2) yes
Cr1 . N3 C9 . 134.69(18) yes
Cr1 . N3 C12 . 114.88(17) yes
C9 . N3 C12 . 109.0(2) yes
Cr1 . N4 C13 . 113.77(17) yes
Cr1 . N4 C14 . 117.22(16) yes
C13 . N4 C14 . 128.8(2) yes
N1 . C1 C2 . 118.2(2) yes
N1 . C1 H11 . 120.9 no
C2 . C1 H11 . 120.9 no
C1 . C2 N2 . 114.6(2) yes
C1 . C2 C3 . 135.4(3) yes
N2 . C2 C3 . 109.7(2) yes
C2 . C3 C4 . 104.8(2) yes
C2 . C3 H31 . 127.6 no
C4 . C3 H31 . 127.6 no
C3 . C4 C5 . 108.0(2) yes
C3 . C4 H41 . 126.0 no
C5 . C4 H41 . 126.0 no
C4 . C5 N2 . 108.6(2) yes
C4 . C5 C6 . 129.3(2) yes
N2 . C5 C6 . 121.9(2) yes
C5 . C6 C7 . 110.4(2) yes
C5 . C6 C8 . 107.0(2) yes
C7 . C6 C8 . 109.8(2) yes
C5 . C6 C9 . 112.0(2) yes
C7 . C6 C9 . 111.0(2) yes
C8 . C6 C9 . 106.4(2) yes
C6 . C7 H71 . 109.5 no
C6 . C7 H72 . 109.5 no
H71 . C7 H72 . 109.5 no
C6 . C7 H73 . 109.3 no
H71 . C7 H73 . 109.5 no
H72 . C7 H73 . 109.5 no
C6 . C8 H81 . 109.5 no
C6 . C8 H82 . 109.5 no
H81 . C8 H82 . 109.5 no
C6 . C8 H83 . 109.4 no
H81 . C8 H83 . 109.5 no
H82 . C8 H83 . 109.5 no
C6 . C9 N3 . 119.9(2) yes
C6 . C9 C10 . 130.7(2) yes
N3 . C9 C10 . 108.9(2) yes
C9 . C10 C11 . 108.0(2) yes
C9 . C10 H101 . 126.0 no
C11 . C10 H101 . 126.1 no
C10 . C11 C12 . 106.3(3) yes
C10 . C11 H111 . 126.8 no
C12 . C11 H111 . 126.9 no
C11 . C12 N3 . 107.9(2) yes
C11 . C12 C13 . 138.2(3) yes
N3 . C12 C13 . 113.5(2) yes
C12 . C13 N4 . 116.4(2) yes
C12 . C13 H131 . 121.8 no
N4 . C13 H131 . 121.8 no
N4 . C14 C21 5_656 115.2(2) yes
N4 . C14 C15 . 125.1(2) yes
C21 5_656 C14 C15 . 119.2(2) yes
C14 . C15 C16 . 120.5(2) yes
C14 . C15 H151 . 119.7 no
C16 . C15 H151 . 119.7 no
C15 . C16 C19 5_656 119.7(2) yes
C15 . C16 C17 . 117.2(3) yes
C19 5_656 C16 C17 . 123.0(3) yes
C16 . C17 H171 . 109.4 no
C16 . C17 H172 . 109.5 no
H171 . C17 H172 . 109.5 no
C16 . C17 H173 . 109.5 no
H171 . C17 H173 . 109.5 no
H172 . C17 H173 . 109.5 no
C19 . C18 H181 . 109.4 no
C19 . C18 H182 . 109.6 no
H181 . C18 H182 . 109.5 no
C19 . C18 H183 . 109.4 no
H181 . C18 H183 . 109.5 no
H182 . C18 H183 . 109.5 no
C18 . C19 C16 5_656 121.8(3) yes
C18 . C19 C20 . 118.4(3) yes
C16 5_656 C19 C20 . 119.9(2) yes
C19 . C20 C21 . 120.3(2) yes
C19 . C20 H201 . 119.9 no
C21 . C20 H201 . 119.8 no
N1 . C21 C14 5_656 120.3(2) yes
N1 . C21 C20 . 119.7(2) yes
C14 5_656 C21 C20 . 119.9(2) yes
C24 4_667 C22 C23 . 119.9(4) yes
C24 4_667 C22 H221 . 120.0 no
C23 . C22 H221 . 120.0 no
C22 . C23 C24 . 119.7(3) yes
C22 . C23 H231 . 120.2 no
C24 . C23 H231 . 120.0 no
C23 . C24 C22 4_667 120.3(4) yes
C23 . C24 H241 . 119.7 no
C22 4_667 C24 H241 . 119.9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cr1 N1 5_656 2.649(2) yes
Cr1 N1 . 2.101(2) yes
Cr1 N2 . 1.964(2) yes
Cr1 N3 . 1.965(2) yes
Cr1 N4 . 2.065(2) yes
N1 C1 . 1.333(3) yes
N1 C21 . 1.423(3) yes
N2 C2 . 1.368(4) yes
N2 C5 . 1.335(4) yes
N3 C9 . 1.337(3) yes
N3 C12 . 1.384(3) yes
N4 C13 . 1.307(3) yes
N4 C14 . 1.402(3) yes
C1 C2 . 1.413(4) yes
C1 H11 . 0.950 no
C2 C3 . 1.401(4) yes
C3 C4 . 1.405(4) yes
C3 H31 . 0.950 no
C4 C5 . 1.401(4) yes
C4 H41 . 0.950 no
C5 C6 . 1.518(4) yes
C6 C7 . 1.509(4) yes
C6 C8 . 1.536(3) yes
C6 C9 . 1.533(3) yes
C7 H71 . 0.950 no
C7 H72 . 0.950 no
C7 H73 . 0.950 no
C8 H81 . 0.950 no
C8 H82 . 0.950 no
C8 H83 . 0.950 no
C9 C10 . 1.394(4) yes
C10 C11 . 1.390(4) yes
C10 H101 . 0.950 no
C11 C12 . 1.409(4) yes
C11 H111 . 0.950 no
C12 C13 . 1.416(4) yes
C13 H131 . 0.950 no
C14 C21 5_656 1.398(3) yes
C14 C15 . 1.394(3) yes
C15 C16 . 1.397(4) yes
C15 H151 . 0.950 no
C16 C19 5_656 1.388(4) yes
C16 C17 . 1.493(4) yes
C17 H171 . 0.950 no
C17 H172 . 0.950 no
C17 H173 . 0.950 no
C18 C19 . 1.506(4) yes
C18 H181 . 0.950 no
C18 H182 . 0.950 no
C18 H183 . 0.950 no
C19 C20 . 1.394(4) yes
C20 C21 . 1.391(4) yes
C20 H201 . 0.950 no
C22 C24 4_667 1.368(6) yes
C22 C23 . 1.391(5) yes
C22 H221 . 0.950 no
C23 C24 . 1.375(6) yes
C23 H231 . 0.950 no
C24 H241 . 0.950 no
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
-1 5 7 x
-9 3 11 x
-6 4 14 x
-7 3 11 x
-18 2 4 x
-12 8 8 x
0 2 10 x
2 6 11 x
2 6 5 x
12 4 9 x
10 4 0 x
12 8 7 x
-2 8 5 x
-6 8 5 x
1 1 7 x
1 5 6 x
12 8 3 x
-3 11 7 x
4 10 7 x
5 1 5 x
2 2 2 x
