#------------------------------------------------------------------------------
#$Date: 2019-11-23 03:21:12 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231990 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/68/4346803.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_4346803
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 0.86 GPa structure'
_audit_creation_date             2014-08-21
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 116.722(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5598(16)
_cell_length_b                   13.2590(15)
_cell_length_c                   15.0110(15)
_cell_measurement_reflns_used    3799
_cell_measurement_temperature    300
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_volume                     3655.0(6)
_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         1600000
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.646
_diffrn_measured_fraction_theta_max 0.646
_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  0.065
_diffrn_reflns_limit_h_max       25
_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            7894
_diffrn_reflns_theta_full        17.722
_diffrn_reflns_theta_max         17.722
_diffrn_reflns_theta_min         2.287
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.524
_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         0.36
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0708
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         1823
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.0005935
_refine_ls_shift/su_mean         0.0000334
_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: 
 0.400 0.203 0.283 0.823E-01 0.177 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0603
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0451
_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                1823
_reflns_number_total             2437
_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   0.0500
_oxford_refine_ls_scale          0.1293(3)
_oxford_reflns_number_all        2418
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'crpak3 in C2/c'
_cod_data_source_file            1_60GPa.cif
_cod_data_source_block           1_60GPa
_cod_original_cell_volume        3655.0(4)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4346803
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 0.58350(2) 0.66409(4) 0.77738(4) 0.0257 1.0000 Uani . .
N1 N 0.54107(13) 0.7300(2) 0.8674(2) 0.0254 1.0000 Uani . U
N2 N 0.58506(12) 0.5465(2) 0.85870(19) 0.0228 1.0000 Uani . U
N3 N 0.64791(12) 0.5837(2) 0.73974(19) 0.0228 1.0000 Uani . U
N4 N 0.60218(12) 0.7640(2) 0.68525(19) 0.0244 1.0000 Uani . U
C1 C 0.54037(14) 0.6641(2) 0.9342(2) 0.0222 1.0000 Uani . U
C2 C 0.56534(14) 0.5653(2) 0.9329(2) 0.0232 1.0000 Uani . U
C3 C 0.58268(16) 0.4814(3) 0.9959(2) 0.0288 1.0000 Uani . U
C4 C 0.61403(16) 0.4107(3) 0.9575(2) 0.0278 1.0000 Uani . U
C5 C 0.61634(14) 0.4554(2) 0.8731(2) 0.0225 1.0000 Uani . U
C6 C 0.64238(14) 0.4117(2) 0.8018(2) 0.0236 1.0000 Uani . U
C7 C 0.69475(17) 0.3244(3) 0.8506(3) 0.0379 1.0000 Uani . U
C8 C 0.57479(16) 0.3723(3) 0.7103(3) 0.0311 1.0000 Uani . U
C9 C 0.67692(14) 0.4921(2) 0.7628(2) 0.0223 1.0000 Uani . U
C10 C 0.73322(15) 0.4839(3) 0.7348(2) 0.0280 1.0000 Uani . U
C11 C 0.73884(15) 0.5757(3) 0.6941(3) 0.0285 1.0000 Uani . U
C12 C 0.68466(14) 0.6394(2) 0.6982(2) 0.0234 1.0000 Uani . U
C13 C 0.65392(13) 0.7347(2) 0.6631(2) 0.0246 1.0000 Uani . U
C14 C 0.55603(14) 0.8484(2) 0.6505(2) 0.0220 1.0000 Uani . U
C15 C 0.57761(16) 0.9460(3) 0.6430(2) 0.0277 1.0000 Uani . U
C16 C 0.53058(17) 1.0272(3) 0.6252(2) 0.0294 1.0000 Uani . U
C17 C 0.5586(2) 1.1308(3) 0.6229(3) 0.0459 1.0000 Uani . U
C18 C 0.5925(2) 1.0947(4) 0.9019(3) 0.0538 1.0000 Uani . U
C19 C 0.53954(17) 1.0094(3) 0.8866(2) 0.0326 1.0000 Uani . U
C20 C 0.56248(16) 0.9110(3) 0.8839(2) 0.0282 1.0000 Uani . U
C21 C 0.51640(14) 0.8303(2) 0.8688(2) 0.0229 1.0000 Uani . U
C22 C 0.7773(2) 0.7685(4) 0.9328(3) 0.0488 1.0000 Uani . U
C23 C 0.76389(19) 0.6708(4) 0.9520(3) 0.0483 1.0000 Uani . U
C24 C 0.7368(2) 0.6524(4) 1.0193(3) 0.0493 1.0000 Uani . U
H11 H 0.5235 0.6834 0.9811 0.0269 1.0000 Uiso R .
H31 H 0.5747 0.4738 1.0531 0.0347 1.0000 Uiso R .
H41 H 0.6307 0.3450 0.9831 0.0333 1.0000 Uiso R .
H71 H 0.7106 0.2976 0.8050 0.0456 1.0000 Uiso R .
H72 H 0.7355 0.3475 0.9087 0.0456 1.0000 Uiso R .
H73 H 0.6704 0.2730 0.8684 0.0456 1.0000 Uiso R .
H81 H 0.5892 0.3441 0.6638 0.0369 1.0000 Uiso R .
H82 H 0.5418 0.4262 0.6800 0.0369 1.0000 Uiso R .
H83 H 0.5516 0.3218 0.7311 0.0369 1.0000 Uiso R .
H101 H 0.7625 0.4259 0.7422 0.0336 1.0000 Uiso R .
H111 H 0.7722 0.5923 0.6687 0.0346 1.0000 Uiso R .
H131 H 0.6702 0.7761 0.6257 0.0296 1.0000 Uiso R .
H151 H 0.6254 0.9574 0.6505 0.0332 1.0000 Uiso R .
H171 H 0.5213 1.1786 0.6101 0.0552 1.0000 Uiso R .
H172 H 0.5989 1.1448 0.6856 0.0552 1.0000 Uiso R .
H173 H 0.5740 1.1342 0.5720 0.0552 1.0000 Uiso R .
H181 H 0.6372 1.0682 0.9083 0.0640 1.0000 Uiso R .
H182 H 0.6008 1.1309 0.9609 0.0640 1.0000 Uiso R .
H183 H 0.5727 1.1394 0.8464 0.0640 1.0000 Uiso R .
H201 H 0.6106 0.8991 0.8926 0.0338 1.0000 Uiso R .
H221 H 0.7963 0.7811 0.8867 0.0591 1.0000 Uiso R .
H231 H 0.7734 0.6165 0.9186 0.0581 1.0000 Uiso R .
H241 H 0.7278 0.5850 1.0327 0.0588 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 . 82.09(11) yes
N1 5_656 Cr1 N2 . 120.57(9) yes
N1 . Cr1 N2 . 80.02(11) yes
N1 5_656 Cr1 N3 . 117.98(10) yes
N1 . Cr1 N3 . 159.53(10) yes
N2 . Cr1 N3 . 85.63(11) yes
N1 5_656 Cr1 N4 . 69.09(8) yes
N1 . Cr1 N4 . 114.74(11) yes
N2 . Cr1 N4 . 164.30(10) yes
N3 . Cr1 N4 . 78.72(11) yes
Cr1 . N1 Cr1 5_656 82.14(9) yes
Cr1 . N1 C1 . 111.0(2) yes
Cr1 5_656 N1 C1 . 93.83(18) yes
Cr1 . N1 C21 . 130.6(2) yes
Cr1 5_656 N1 C21 . 95.78(16) yes
C1 . N1 C21 . 118.3(3) yes
Cr1 . N2 C2 . 115.6(2) yes
Cr1 . N2 C5 . 133.3(2) yes
C2 . N2 C5 . 109.2(2) yes
Cr1 . N3 C9 . 134.5(2) yes
Cr1 . N3 C12 . 114.4(2) yes
C9 . N3 C12 . 109.4(2) yes
Cr1 . N4 C13 . 113.3(2) yes
Cr1 . N4 C14 . 117.36(19) yes
C13 . N4 C14 . 129.2(3) yes
N1 . C1 C2 . 118.1(3) yes
N1 . C1 H11 . 120.8 no
C2 . C1 H11 . 121.1 no
C1 . C2 N2 . 115.1(3) yes
C1 . C2 C3 . 135.5(3) yes
N2 . C2 C3 . 109.1(3) yes
C2 . C3 C4 . 106.1(3) yes
C2 . C3 H31 . 127.0 no
C4 . C3 H31 . 126.9 no
C3 . C4 C5 . 107.1(3) yes
C3 . C4 H41 . 126.5 no
C5 . C4 H41 . 126.3 no
C4 . C5 N2 . 108.4(3) yes
C4 . C5 C6 . 129.6(3) yes
N2 . C5 C6 . 121.9(3) yes
C5 . C6 C7 . 110.4(3) yes
C5 . C6 C8 . 107.2(2) yes
C7 . C6 C8 . 109.3(3) yes
C5 . C6 C9 . 112.0(3) yes
C7 . C6 C9 . 111.3(2) yes
C8 . C6 C9 . 106.4(3) yes
C6 . C7 H71 . 109.5 no
C6 . C7 H72 . 109.8 no
H71 . C7 H72 . 109.6 no
C6 . C7 H73 . 109.3 no
H71 . C7 H73 . 109.3 no
H72 . C7 H73 . 109.4 no
C6 . C8 H81 . 109.6 no
C6 . C8 H82 . 109.7 no
H81 . C8 H82 . 109.6 no
C6 . C8 H83 . 109.3 no
H81 . C8 H83 . 109.3 no
H82 . C8 H83 . 109.4 no
C6 . C9 N3 . 120.3(3) yes
C6 . C9 C10 . 130.2(3) yes
N3 . C9 C10 . 109.1(3) yes
C9 . C10 C11 . 107.9(3) yes
C9 . C10 H101 . 126.3 no
C11 . C10 H101 . 125.9 no
C10 . C11 C12 . 106.3(3) yes
C10 . C11 H111 . 126.8 no
C12 . C11 H111 . 127.0 no
C11 . C12 N3 . 107.4(3) yes
C11 . C12 C13 . 138.4(3) yes
N3 . C12 C13 . 113.8(3) yes
C12 . C13 N4 . 116.9(3) yes
C12 . C13 H131 . 121.6 no
N4 . C13 H131 . 121.5 no
N4 . C14 C21 5_656 114.6(3) yes
N4 . C14 C15 . 125.8(3) yes
C21 5_656 C14 C15 . 119.4(3) yes
C14 . C15 C16 . 121.1(3) yes
C14 . C15 H151 . 119.4 no
C16 . C15 H151 . 119.5 no
C19 5_656 C16 C15 . 119.0(3) yes
C19 5_656 C16 C17 . 122.7(3) yes
C15 . C16 C17 . 118.3(3) yes
C16 . C17 H171 . 109.5 no
C16 . C17 H172 . 109.2 no
H171 . C17 H172 . 109.8 no
C16 . C17 H173 . 109.3 no
H171 . C17 H173 . 109.8 no
H172 . C17 H173 . 109.2 no
C19 . C18 H181 . 109.8 no
C19 . C18 H182 . 109.4 no
H181 . C18 H182 . 109.4 no
C19 . C18 H183 . 109.6 no
H181 . C18 H183 . 109.6 no
H182 . C18 H183 . 109.0 no
C18 . C19 C16 5_656 121.8(4) yes
C18 . C19 C20 . 118.3(3) yes
C16 5_656 C19 C20 . 120.0(3) yes
C19 . C20 C21 . 121.0(3) yes
C19 . C20 H201 . 119.7 no
C21 . C20 H201 . 119.3 no
N1 . C21 C14 5_656 120.5(3) yes
N1 . C21 C20 . 120.2(3) yes
C14 5_656 C21 C20 . 119.2(3) yes
C24 4_667 C22 C23 . 119.8(5) yes
C24 4_667 C22 H221 . 120.0 no
C23 . C22 H221 . 120.3 no
C22 . C23 C24 . 120.3(4) yes
C22 . C23 H231 . 119.6 no
C24 . C23 H231 . 120.1 no
C23 . C24 C22 4_667 119.9(5) yes
C23 . C24 H241 . 120.2 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 2.653(3) yes
Cr1 N1 . 2.100(3) yes
Cr1 N2 . 1.971(3) yes
Cr1 N3 . 1.970(3) yes
Cr1 N4 . 2.072(3) yes
N1 C1 . 1.335(4) yes
N1 C21 . 1.426(4) yes
N2 C2 . 1.368(4) yes
N2 C5 . 1.340(4) yes
N3 C9 . 1.328(4) yes
N3 C12 . 1.389(4) yes
N4 C13 . 1.308(4) yes
N4 C14 . 1.407(4) yes
C1 C2 . 1.410(4) yes
C1 H11 . 0.951 no
C2 C3 . 1.400(5) yes
C3 C4 . 1.401(5) yes
C3 H31 . 0.948 no
C4 C5 . 1.418(5) yes
C4 H41 . 0.951 no
C5 C6 . 1.512(4) yes
C6 C7 . 1.526(4) yes
C6 C8 . 1.540(4) yes
C6 C9 . 1.535(4) yes
C7 H71 . 0.950 no
C7 H72 . 0.948 no
C7 H73 . 0.952 no
C8 H81 . 0.950 no
C8 H82 . 0.949 no
C8 H83 . 0.953 no
C9 C10 . 1.403(4) yes
C10 C11 . 1.389(5) yes
C10 H101 . 0.952 no
C11 C12 . 1.421(4) yes
C11 H111 . 0.950 no
C12 C13 . 1.406(5) yes
C13 H131 . 0.947 no
C14 C21 5_656 1.404(4) yes
C14 C15 . 1.389(4) yes
C15 C16 . 1.391(5) yes
C15 H151 . 0.950 no
C16 C19 5_656 1.392(5) yes
C16 C17 . 1.496(5) yes
C17 H171 . 0.945 no
C17 H172 . 0.952 no
C17 H173 . 0.952 no
C18 C19 . 1.514(5) yes
C18 H181 . 0.947 no
C18 H182 . 0.954 no
C18 H183 . 0.951 no
C19 C20 . 1.395(5) yes
C20 C21 . 1.379(4) yes
C20 H201 . 0.951 no
C22 C24 4_667 1.375(7) yes
C22 C23 . 1.382(6) yes
C22 H221 . 0.949 no
C23 C24 . 1.377(6) yes
C23 H231 . 0.947 no
C24 H241 . 0.952 no
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
-9 3 11 x
-6 4 4 x
5 3 14 x
4 0 4 x
-12 8 8 x
14 8 1 x
-3 3 14 x
5 9 6 x
9 5 4 x
-5 3 11 x
-5 9 11 x
6 8 8 x
1 7 11 x
-3 11 8 x
-11 7 7 x
-20 2 4 x
4 10 7 x
4 8 6 x
-18 6 4 x
