#------------------------------------------------------------------------------
#$Date: 2019-11-23 03:22:03 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231994 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/68/4346807.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_4346807
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 0.137 GPa structure'
_audit_creation_date             2014-08-21
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 115.640(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7681(19)
_cell_length_b                   13.3809(16)
_cell_length_c                   15.2439(17)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    300
_cell_measurement_theta_max      17
_cell_measurement_theta_min      3
_cell_volume                     3819.1(7)
_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         860000
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.666
_diffrn_measured_fraction_theta_max 0.666
_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  0.059
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7557
_diffrn_reflns_theta_full        15.672
_diffrn_reflns_theta_max         15.672
_diffrn_reflns_theta_min         2.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.459
_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         0.39
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         1423
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.0005472
_refine_ls_shift/su_mean         0.0000359
_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: 
 0.485 0.433 0.408 0.217 0.223 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0652
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0434
_reflns_limit_h_max              20
_reflns_limit_h_min              -22
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1423
_reflns_number_total             1834
_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   0.0526
_oxford_refine_ls_scale          0.1059(3)
_oxford_reflns_number_all        1812
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'crpak2_0m in C2/c'
_cod_data_source_file            0_86GPa.cif
_cod_data_source_block           0_86GPa
_cod_original_cell_volume        3819.1(4)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4346807
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 0.58209(3) 0.66166(5) 0.77632(5) 0.0273 1.0000 Uani . .
N1 N 0.54040(17) 0.7279(3) 0.8662(3) 0.0268 1.0000 Uani . U
N2 N 0.58450(16) 0.5451(3) 0.8575(2) 0.0248 1.0000 Uani . U
N3 N 0.64598(16) 0.5829(3) 0.7383(2) 0.0246 1.0000 Uani . U
N4 N 0.60066(17) 0.7616(3) 0.6857(3) 0.0274 1.0000 Uani . U
C1 C 0.54078(19) 0.6623(3) 0.9322(3) 0.0249 1.0000 Uani . U
C2 C 0.56503(19) 0.5647(3) 0.9310(3) 0.0236 1.0000 Uani . U
C3 C 0.5825(2) 0.4809(3) 0.9931(3) 0.0302 1.0000 Uani . U
C4 C 0.6146(2) 0.4121(3) 0.9546(3) 0.0335 1.0000 Uani . U
C5 C 0.61592(19) 0.4552(3) 0.8721(3) 0.0261 1.0000 Uani . U
C6 C 0.6418(2) 0.4123(3) 0.8010(3) 0.0277 1.0000 Uani . U
C7 C 0.6948(2) 0.3273(3) 0.8486(4) 0.0419 1.0000 Uani . U
C8 C 0.5764(2) 0.3713(3) 0.7128(3) 0.0369 1.0000 Uani . U
C9 C 0.6754(2) 0.4924(3) 0.7613(3) 0.0231 1.0000 Uani . U
C10 C 0.7312(2) 0.4854(3) 0.7335(3) 0.0329 1.0000 Uani . U
C11 C 0.7360(2) 0.5766(3) 0.6929(3) 0.0332 1.0000 Uani . U
C12 C 0.68200(19) 0.6384(3) 0.6964(3) 0.0256 1.0000 Uani . U
C13 C 0.6521(2) 0.7332(3) 0.6638(3) 0.0276 1.0000 Uani . U
C14 C 0.5550(2) 0.8453(3) 0.6515(3) 0.0235 1.0000 Uani . U
C15 C 0.5765(2) 0.9415(3) 0.6456(3) 0.0309 1.0000 Uani . U
C16 C 0.5296(2) 1.0219(3) 0.6256(3) 0.0348 1.0000 Uani . U
C17 C 0.5569(3) 1.1256(4) 0.6223(4) 0.0537 1.0000 Uani . U
C18 C 0.5932(3) 1.0879(4) 0.9056(5) 0.0599 1.0000 Uani . U
C19 C 0.5409(2) 1.0039(3) 0.8891(3) 0.0361 1.0000 Uani . U
C20 C 0.5624(2) 0.9062(3) 0.8854(3) 0.0300 1.0000 Uani . U
C21 C 0.5165(2) 0.8274(3) 0.8690(3) 0.0256 1.0000 Uani . U
C22 C 0.7753(3) 0.7684(5) 0.9323(4) 0.0575 1.0000 Uani . U
C23 C 0.7613(3) 0.6725(5) 0.9492(4) 0.0586 1.0000 Uani . U
C24 C 0.7351(3) 0.6540(4) 1.0169(4) 0.0586 1.0000 Uani . U
H11 H 0.5249 0.6815 0.9796 0.0299 1.0000 Uiso R .
H31 H 0.5744 0.4728 1.0495 0.0357 1.0000 Uiso R .
H41 H 0.6321 0.3477 0.9801 0.0400 1.0000 Uiso R .
H71 H 0.7106 0.3011 0.8033 0.0502 1.0000 Uiso R .
H72 H 0.7347 0.3520 0.9040 0.0502 1.0000 Uiso R .
H73 H 0.6721 0.2759 0.8681 0.0502 1.0000 Uiso R .
H81 H 0.5914 0.3439 0.6672 0.0439 1.0000 Uiso R .
H82 H 0.5435 0.4240 0.6831 0.0439 1.0000 Uiso R .
H83 H 0.5541 0.3208 0.7339 0.0439 1.0000 Uiso R .
H101 H 0.7607 0.4287 0.7413 0.0390 1.0000 Uiso R .
H111 H 0.7691 0.5938 0.6676 0.0392 1.0000 Uiso R .
H131 H 0.6685 0.7749 0.6273 0.0326 1.0000 Uiso R .
H151 H 0.6242 0.9532 0.6553 0.0372 1.0000 Uiso R .
H171 H 0.5194 1.1726 0.6081 0.0648 1.0000 Uiso R .
H172 H 0.5951 1.1412 0.6835 0.0648 1.0000 Uiso R .
H173 H 0.5733 1.1284 0.5731 0.0648 1.0000 Uiso R .
H181 H 0.6380 1.0612 0.9143 0.0722 1.0000 Uiso R .
H182 H 0.5990 1.1245 0.9619 0.0722 1.0000 Uiso R .
H183 H 0.5755 1.1309 0.8506 0.0722 1.0000 Uiso R .
H201 H 0.6099 0.8939 0.8944 0.0363 1.0000 Uiso R .
H221 H 0.7926 0.7813 0.8851 0.0689 1.0000 Uiso R .
H231 H 0.7694 0.6187 0.9146 0.0701 1.0000 Uiso R .
H241 H 0.7246 0.5875 1.0284 0.0699 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 . Cr1 N2 . 80.29(14) yes
N1 . Cr1 N3 . 159.38(13) yes
N2 . Cr1 N3 . 85.65(14) yes
N1 . Cr1 N4 . 114.11(14) yes
N2 . Cr1 N4 . 164.34(13) yes
N3 . Cr1 N4 . 78.82(14) yes
Cr1 . N1 C1 . 110.1(3) yes
Cr1 . N1 C21 . 131.1(3) yes
C1 . N1 C21 . 118.7(4) yes
Cr1 . N2 C2 . 115.1(3) yes
Cr1 . N2 C5 . 133.7(3) yes
C2 . N2 C5 . 109.2(3) yes
Cr1 . N3 C9 . 134.4(3) yes
Cr1 . N3 C12 . 114.5(3) yes
C9 . N3 C12 . 109.3(3) yes
Cr1 . N4 C13 . 113.0(3) yes
Cr1 . N4 C14 . 117.9(3) yes
C13 . N4 C14 . 129.0(4) yes
N1 . C1 C2 . 119.2(4) yes
N1 . C1 H11 . 120.4 no
C2 . C1 H11 . 120.4 no
C1 . C2 N2 . 115.0(3) yes
C1 . C2 C3 . 136.1(4) yes
N2 . C2 C3 . 108.5(4) yes
C2 . C3 C4 . 105.7(4) yes
C2 . C3 H31 . 127.1 no
C4 . C3 H31 . 127.1 no
C3 . C4 C5 . 107.7(4) yes
C3 . C4 H41 . 126.2 no
C5 . C4 H41 . 126.2 no
C4 . C5 N2 . 108.9(4) yes
C4 . C5 C6 . 129.8(4) yes
N2 . C5 C6 . 121.2(4) yes
C5 . C6 C7 . 110.3(4) yes
C5 . C6 C8 . 107.9(3) yes
C7 . C6 C8 . 109.3(4) yes
C5 . C6 C9 . 112.3(4) yes
C7 . C6 C9 . 110.4(3) yes
C8 . C6 C9 . 106.5(4) yes
C6 . C7 H71 . 109.4 no
C6 . C7 H72 . 109.5 no
H71 . C7 H72 . 109.5 no
C6 . C7 H73 . 109.5 no
H71 . C7 H73 . 109.5 no
H72 . C7 H73 . 109.5 no
C6 . C8 H81 . 109.4 no
C6 . C8 H82 . 109.5 no
H81 . C8 H82 . 109.5 no
C6 . C8 H83 . 109.5 no
H81 . C8 H83 . 109.5 no
H82 . C8 H83 . 109.5 no
C6 . C9 N3 . 120.2(3) yes
C6 . C9 C10 . 130.4(4) yes
N3 . C9 C10 . 109.0(4) yes
C9 . C10 C11 . 107.7(4) yes
C9 . C10 H101 . 126.1 no
C11 . C10 H101 . 126.2 no
C10 . C11 C12 . 106.6(4) yes
C10 . C11 H111 . 126.6 no
C12 . C11 H111 . 126.7 no
C11 . C12 N3 . 107.4(4) yes
C11 . C12 C13 . 138.8(4) yes
N3 . C12 C13 . 113.6(3) yes
C12 . C13 N4 . 117.3(4) yes
C12 . C13 H131 . 121.4 no
N4 . C13 H131 . 121.3 no
N4 . C14 C21 5_656 115.1(3) yes
N4 . C14 C15 . 125.5(4) yes
C21 5_656 C14 C15 . 119.2(4) yes
C14 . C15 C16 . 121.4(4) yes
C14 . C15 H151 . 119.3 no
C16 . C15 H151 . 119.4 no
C19 5_656 C16 C15 . 119.0(4) yes
C19 5_656 C16 C17 . 122.3(4) yes
C15 . C16 C17 . 118.7(4) yes
C16 . C17 H171 . 109.4 no
C16 . C17 H172 . 109.6 no
H171 . C17 H172 . 109.5 no
C16 . C17 H173 . 109.4 no
H171 . C17 H173 . 109.5 no
H172 . C17 H173 . 109.5 no
C19 . C18 H181 . 109.5 no
C19 . C18 H182 . 109.6 no
H181 . C18 H182 . 109.5 no
C19 . C18 H183 . 109.3 no
H181 . C18 H183 . 109.5 no
H182 . C18 H183 . 109.5 no
C18 . C19 C16 5_656 121.8(5) yes
C18 . C19 C20 . 119.1(5) yes
C16 5_656 C19 C20 . 119.1(4) yes
C19 . C20 C21 . 121.3(4) yes
C19 . C20 H201 . 119.3 no
C21 . C20 H201 . 119.3 no
N1 . C21 C14 5_656 120.1(3) yes
N1 . C21 C20 . 119.9(4) yes
C14 5_656 C21 C20 . 119.8(4) yes
C24 4_667 C22 C23 . 120.6(6) yes
C24 4_667 C22 H221 . 119.7 no
C23 . C22 H221 . 119.8 no
C22 . C23 C24 . 119.7(5) yes
C22 . C23 H231 . 120.2 no
C24 . C23 H231 . 120.1 no
C23 . C24 C22 4_667 119.8(6) yes
C23 . C24 H241 . 120.1 no
C22 4_667 C24 H241 . 120.1 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 . 2.106(4) yes
Cr1 N2 . 1.977(4) yes
Cr1 N3 . 1.967(3) yes
Cr1 N4 . 2.075(3) yes
N1 C1 . 1.333(6) yes
N1 C21 . 1.429(5) yes
N2 C2 . 1.371(5) yes
N2 C5 . 1.341(5) yes
N3 C9 . 1.333(5) yes
N3 C12 . 1.391(5) yes
N4 C13 . 1.306(5) yes
N4 C14 . 1.413(5) yes
C1 C2 . 1.404(6) yes
C1 H11 . 0.950 no
C2 C3 . 1.409(6) yes
C3 C4 . 1.406(6) yes
C3 H31 . 0.950 no
C4 C5 . 1.395(6) yes
C4 H41 . 0.950 no
C5 C6 . 1.516(6) yes
C6 C7 . 1.531(6) yes
C6 C8 . 1.540(6) yes
C6 C9 . 1.538(6) 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 . 1.400(6) yes
C10 C11 . 1.391(6) yes
C10 H101 . 0.950 no
C11 C12 . 1.413(6) yes
C11 H111 . 0.950 no
C12 C13 . 1.405(6) yes
C13 H131 . 0.950 no
C14 C21 5_656 1.399(5) yes
C14 C15 . 1.378(6) yes
C15 C16 . 1.394(6) yes
C15 H151 . 0.950 no
C16 C19 5_656 1.402(7) yes
C16 C17 . 1.508(6) yes
C17 H171 . 0.950 no
C17 H172 . 0.950 no
C17 H173 . 0.950 no
C18 C19 . 1.507(6) yes
C18 H181 . 0.950 no
C18 H182 . 0.950 no
C18 H183 . 0.950 no
C19 C20 . 1.391(6) yes
C20 C21 . 1.370(6) yes
C20 H201 . 0.950 no
C22 C24 4_667 1.368(9) yes
C22 C23 . 1.364(8) yes
C22 H221 . 0.950 no
C23 C24 . 1.382(9) 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
-6 4 4 x
-4 4 5 x
2 0 10 x
1 3 5 x
11 3 0 x
2 2 5 x
-15 3 7 x
10 2 7 x
17 3 2 x
4 2 4 x
-9 9 11 x
10 10 1 x
4 8 5 x
0 0 6 x
-5 9 2 x
6 2 1 x
-2 6 4 x
10 2 2 x
-6 10 10 x
-2 2 11 x
7 7 4 x
-1 1 11 x
