data_7
_audit_creation_date              2017-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790;
Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984;
Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45,
 575-580.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common             ?
_chemical_name_systematic
;
 ? 
;
_chemical_formula_moiety          'I, 2(C6 H16 Cl Cr0.5 N2), C4 H8 O'
_chemical_formula_sum             'C16 H40 Cl2 Cr I N4 O'
_chemical_formula_weight          554.32
_chemical_melting_point           ?
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'
 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I' 'I' -0.4742 1.8119 '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'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system       'monoclinic'
_space_group_IT_number            13
_space_group_name_H-M_alt         'P 1 2/c 1'
_space_group_name_Hall            '-P 2yc'
loop_
  _space_group_symop_id
  _space_group_symop_operation_xyz
 1 'x, y, z'
 2 '-x, y, -z+1/2'
 3 '-x, -y, -z'
 4 'x, -y, z-1/2'

_cell_length_a                    11.379(2)
_cell_length_b                    11.659(2)
_cell_length_c                    18.521(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  102.867(4)
_cell_angle_gamma                 90.00
_cell_volume                      2395.5(8)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     2497
_cell_measurement_temperature     100
_cell_measurement_theta_max       26.114
_cell_measurement_theta_min       2.256
_exptl_absorpt_coefficient_mu     2.001
_exptl_absorpt_correction_T_max   0.7453
_exptl_absorpt_correction_T_min   0.5760
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1147 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.7728. The λ/2 correction factor is Not present.'
_exptl_crystal_colour             'clear light green'
_exptl_crystal_colour_lustre      clear
_exptl_crystal_colour_modifier    light
_exptl_crystal_colour_primary     green
_exptl_crystal_density_diffrn     1.537
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              1132
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.01
_exptl_special_details
;
 ? 
;
_diffrn_reflns_av_R_equivalents   0.1572
_diffrn_reflns_av_unetI/netI      0.1732
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_number             20541
_diffrn_reflns_theta_full         26.15
_diffrn_reflns_theta_max          26.15
_diffrn_reflns_theta_min          1.75
_diffrn_ambient_temperature       100
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    'fine-focus sealed tube'
_diffrn_special_details           ?
_diffrn_standards_number          0
_reflns_number_gt                 3009
_reflns_number_total              4769
_reflns_threshold_expression      >2sigma(I)
_computing_cell_refinement        'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_data_collection        ?
_computing_data_reduction         'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max          2.357
_refine_diff_density_min          -1.768
_refine_diff_density_rms          0.207
_refine_ls_extinction_coef        ?
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.131
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      236
_refine_ls_number_reflns          4769
_refine_ls_number_restraints      36
_refine_ls_R_factor_all           0.1768
_refine_ls_R_factor_gt            0.1002
_refine_ls_restrained_S_all       1.128
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0512P)²+2.5386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1315
_refine_ls_wR_factor_ref          0.1499
_refine_special_details
'Crystals were twinned resulting in poor data, ISOR command used on NPD atoms.'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      iterative
_atom_sites_solution_secondary    difmap
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_calc_flag
  _atom_site_disorder_assembly
  _atom_site_disorder_group
  _atom_site_site_symmetry_order
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
 I1 I 0.43029(5) 0.26605(5) 0.56305(3) 0.01182(19) Uani 1 d . . 1 . . .
 Cr1 Cr 1.0000 0.26303(16) 0.7500 0.0096(5) Uani 1 d . . 2 S T P
 Cl1 Cl 1.0000 0.0657(2) 0.7500 0.0177(8) Uani 1 d . . 2 S T P
 Cl2 Cl 1.0000 0.4604(2) 0.7500 0.0160(8) Uani 1 d . . 2 S T P
 N1 N 1.1233(6) 0.2621(6) 0.6731(4) 0.0123(16) Uani 1 d . . 1 . . .
 N2 N 0.8315(6) 0.2653(6) 0.6630(4) 0.0127(16) Uani 1 d . . 1 . U .
 C1 C 1.1356(9) 0.3709(8) 0.6332(6) 0.029(3) Uani 1 d . . 1 . . .
 H1A H 1.0573 0.3920 0.6018 0.043 Uiso 1 calc . . 1 GR . .
 H1B H 1.1943 0.3603 0.6022 0.043 Uiso 1 calc . . 1 GR . .
 H1C H 1.1633 0.4321 0.6692 0.043 Uiso 1 calc . . 1 GR . .
 C2 C 1.1019(9) 0.1699(8) 0.6150(6) 0.032(3) Uani 1 d . . 1 . . .
 H2A H 1.0896 0.0963 0.6378 0.048 Uiso 1 calc . . 1 GR . .
 H2B H 1.1720 0.1643 0.5926 0.048 Uiso 1 calc . . 1 GR . .
 H2C H 1.0302 0.1888 0.5766 0.048 Uiso 1 calc . . 1 GR . .
 C3 C 0.7590(8) 0.2369(8) 0.7760(5) 0.023(2) Uani 1 d . . 1 . . .
 H3A H 0.7537 0.1534 0.7659 0.028 Uiso 1 calc . . 1 R . .
 H3B H 0.6934 0.2574 0.8008 0.028 Uiso 1 calc . . 1 R . .
 C4 C 0.7407(9) 0.2978(10) 0.7061(6) 0.035(3) Uani 1 d . . 1 . . .
 H4A H 0.7457 0.3814 0.7159 0.042 Uiso 1 calc . . 1 R . .
 H4B H 0.6589 0.2809 0.6764 0.042 Uiso 1 calc . . 1 R . .
 C5 C 0.7945(9) 0.1581(8) 0.6223(6) 0.033(3) Uani 1 d . . 1 . . .
 H5A H 0.8547 0.1368 0.5942 0.049 Uiso 1 calc . . 1 GR . .
 H5B H 0.7162 0.1693 0.5881 0.049 Uiso 1 calc . . 1 GR . .
 H5C H 0.7879 0.0969 0.6574 0.049 Uiso 1 calc . . 1 GR . .
 C6 C 0.8205(9) 0.3535(8) 0.6035(6) 0.032(3) Uani 1 d . . 1 . . .
 H6A H 0.8466 0.4281 0.6258 0.049 Uiso 1 calc . . 1 GR . .
 H6B H 0.7364 0.3585 0.5762 0.049 Uiso 1 calc . . 1 GR . .
 H6C H 0.8715 0.3318 0.5695 0.049 Uiso 1 calc . . 1 GR . .
 Cr2 Cr 0.5000 0.23423(16) 0.2500 0.0094(4) Uani 1 d . . 2 S T P
 Cl3 Cl 0.70453(18) 0.23392(18) 0.25809(12) 0.0163(5) Uani 1 d . . 1 . . .
 N3 N 0.5197(6) 0.0921(6) 0.3319(4) 0.0129(18) Uani 1 d . . 1 . . .
 N4 N 0.5221(6) 0.3755(6) 0.3324(4) 0.0126(19) Uani 1 d . . 1 . . .
 C7 C 0.6444(8) 0.0649(8) 0.3748(6) 0.025(3) Uani 1 d . . 1 . U .
 H7A H 0.6969 0.0509 0.3403 0.037 Uiso 1 calc . . 1 GR . .
 H7B H 0.6422 -0.0036 0.4050 0.037 Uiso 1 calc . . 1 GR . .
 H7C H 0.6758 0.1298 0.4070 0.037 Uiso 1 calc . . 1 GR . .
 C8 C 0.4446(9) 0.0991(7) 0.3867(6) 0.022(3) Uani 1 d . . 1 . . .
 H8A H 0.4771 0.1579 0.4235 0.032 Uiso 1 calc . . 1 GR . .
 H8B H 0.4448 0.0247 0.4114 0.032 Uiso 1 calc . . 1 GR . .
 H8C H 0.3619 0.1192 0.3618 0.032 Uiso 1 calc . . 1 GR . .
 C9 C 0.4767(9) -0.0093(7) 0.2842(6) 0.023(2) Uani 1 d . . 1 . U .
 H9A H 0.5030 -0.0803 0.3125 0.027 Uiso 1 calc . . 1 R . .
 H9B H 0.3875 -0.0091 0.2709 0.027 Uiso 1 calc . . 1 R . .
 C10 C 0.4167(8) 0.4028(7) 0.3649(5) 0.016(2) Uani 1 d . . 1 . U .
 H10A H 0.3469 0.4213 0.3251 0.024 Uiso 1 calc . . 1 GR . .
 H10B H 0.4361 0.4687 0.3983 0.024 Uiso 1 calc . . 1 GR . .
 H10C H 0.3978 0.3364 0.3927 0.024 Uiso 1 calc . . 1 GR . .
 C11 C 0.6267(8) 0.3678(8) 0.3968(5) 0.020(2) Uani 1 d . . 1 . U .
 H11A H 0.6089 0.3124 0.4327 0.031 Uiso 1 calc . . 1 GR . .
 H11B H 0.6420 0.4433 0.4203 0.031 Uiso 1 calc . . 1 GR . .
 H11C H 0.6982 0.3427 0.3798 0.031 Uiso 1 calc . . 1 GR . .
 C12 C 0.5438(8) 0.4756(7) 0.2862(5) 0.016(2) Uani 1 d . . 1 . U .
 H12A H 0.5360 0.5479 0.3128 0.019 Uiso 1 calc . . 1 R . .
 H12B H 0.6267 0.4716 0.2781 0.019 Uiso 1 calc . . 1 R . .
 O1 O -0.0627(5) 0.2441(5) 0.4455(3) 0.0236(16) Uani 1 d . . 1 . . .
 C13 C -0.0245(9) 0.1422(8) 0.4133(6) 0.027(3) Uani 1 d . . 1 . . .
 H13A H -0.0802 0.1242 0.3655 0.032 Uiso 1 calc . . 1 R . .
 H13B H -0.0215 0.0758 0.4470 0.032 Uiso 1 calc . . 1 R . .
 C14 C 0.1008(9) 0.1707(9) 0.4020(6) 0.032(3) Uani 1 d . . 1 . . .
 H14A H 0.1638 0.1435 0.4443 0.038 Uiso 1 calc . . 1 R . .
 H14B H 0.1143 0.1351 0.3560 0.038 Uiso 1 calc . . 1 R . .
 C15 C 0.1022(10) 0.2996(9) 0.3967(7) 0.044(4) Uani 1 d . . 1 . . .
 H15A H 0.1108 0.3242 0.3470 0.053 Uiso 1 calc . . 1 R . .
 H15B H 0.1694 0.3322 0.4344 0.053 Uiso 1 calc . . 1 R . .
 C16 C -0.0184(9) 0.3373(8) 0.4106(6) 0.028(3) Uani 1 d . . 1 . . .
 H16A H -0.0083 0.4059 0.4429 0.033 Uiso 1 calc . . 1 R . .
 H16B H -0.0750 0.3562 0.3633 0.033 Uiso 1 calc . . 1 R . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Cr1 Cl1 2.301(3) . ?
 Cr1 Cl2 2.301(3) . ?
 Cr1 N1 2.211(7) . ?
 Cr1 N1 2.211(7) 2_756 ?
 Cr1 N2 2.213(7) . ?
 Cr1 N2 2.213(7) 2_756 ?
 N1 C1 1.491(10) . ?
 N1 C2 1.502(11) . ?
 N1 C3 1.487(11) 2_756 ?
 N2 C4 1.489(11) . ?
 N2 C5 1.472(11) . ?
 N2 C6 1.492(12) . ?
 C3 N1 1.487(11) 2_756 ?
 C3 C4 1.450(13) . ?
 Cr2 Cl3 2.299(2) . ?
 Cr2 Cl3 2.299(2) 2_655 ?
 Cr2 N3 2.224(7) 2_655 ?
 Cr2 N3 2.224(7) . ?
 Cr2 N4 2.222(7) 2_655 ?
 Cr2 N4 2.222(7) . ?
 N3 C7 1.498(11) . ?
 N3 C8 1.467(11) . ?
 N3 C9 1.491(11) . ?
 N4 C10 1.491(10) . ?
 N4 C11 1.488(11) . ?
 N4 C12 1.500(11) . ?
 C9 C9 1.480(18) 2_655 ?
 C12 C12 1.482(17) 2_655 ?
 O1 C13 1.440(11) . ?
 O1 C16 1.414(10) . ?
 C13 C14 1.524(13) . ?
 C14 C15 1.506(14) . ?
 C15 C16 1.517(13) . ?

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
  _geom_angle_publ_flag
 Cl2 Cr1 Cl1 180.000(1) . . ?
 N1 Cr1 Cl1 89.72(18) 2_756 . ?
 N1 Cr1 Cl1 89.72(18) . . ?
 N1 Cr1 Cl2 90.28(18) . . ?
 N1 Cr1 Cl2 90.28(18) 2_756 . ?
 N1 Cr1 N1 179.4(4) . 2_756 ?
 N1 Cr1 N2 95.8(2) 2_756 2_756 ?
 N1 Cr1 N2 84.2(3) . 2_756 ?
 N1 Cr1 N2 95.9(2) . . ?
 N1 Cr1 N2 84.2(3) 2_756 . ?
 N2 Cr1 Cl1 90.69(18) . . ?
 N2 Cr1 Cl1 90.69(18) 2_756 . ?
 N2 Cr1 Cl2 89.31(18) 2_756 . ?
 N2 Cr1 Cl2 89.31(18) . . ?
 N2 Cr1 N2 178.6(4) . 2_756 ?
 C1 N1 Cr1 117.3(5) . . ?
 C1 N1 C2 105.8(7) . . ?
 C2 N1 Cr1 116.1(5) . . ?
 C3 N1 Cr1 101.7(5) 2_756 . ?
 C3 N1 C1 108.2(7) 2_756 . ?
 C3 N1 C2 107.0(7) 2_756 . ?
 C4 N2 Cr1 101.8(6) . . ?
 C4 N2 C6 105.5(7) . . ?
 C5 N2 Cr1 117.7(6) . . ?
 C5 N2 C4 109.7(7) . . ?
 C5 N2 C6 103.9(7) . . ?
 C6 N2 Cr1 117.5(6) . . ?
 C4 C3 N1 113.6(8) . 2_756 ?
 C3 C4 N2 112.0(8) . . ?
 Cl3 Cr2 Cl3 179.82(14) 2_655 . ?
 N3 Cr2 Cl3 90.44(19) 2_655 2_655 ?
 N3 Cr2 Cl3 89.42(19) . 2_655 ?
 N3 Cr2 Cl3 90.45(19) . . ?
 N3 Cr2 Cl3 89.42(19) 2_655 . ?
 N3 Cr2 N3 83.7(4) . 2_655 ?
 N4 Cr2 Cl3 90.22(19) 2_655 . ?
 N4 Cr2 Cl3 90.23(19) . 2_655 ?
 N4 Cr2 Cl3 89.91(19) . . ?
 N4 Cr2 Cl3 89.91(19) 2_655 2_655 ?
 N4 Cr2 N3 96.0(2) 2_655 2_655 ?
 N4 Cr2 N3 179.3(3) . 2_655 ?
 N4 Cr2 N3 96.0(2) . . ?
 N4 Cr2 N3 179.3(3) 2_655 . ?
 N4 Cr2 N4 84.3(4) . 2_655 ?
 C7 N3 Cr2 117.3(5) . . ?
 C8 N3 Cr2 116.4(5) . . ?
 C8 N3 C7 105.9(8) . . ?
 C8 N3 C9 106.8(7) . . ?
 C9 N3 Cr2 102.5(6) . . ?
 C9 N3 C7 107.1(7) . . ?
 C10 N4 Cr2 117.2(5) . . ?
 C10 N4 C12 108.3(7) . . ?
 C11 N4 Cr2 117.0(5) . . ?
 C11 N4 C10 105.2(7) . . ?
 C11 N4 C12 107.5(7) . . ?
 C12 N4 Cr2 101.1(5) . . ?
 C9 C9 N3 112.0(6) 2_655 . ?
 C12 C12 N4 110.7(6) 2_655 . ?
 C16 O1 C13 105.8(7) . . ?
 O1 C13 C14 104.8(8) . . ?
 C15 C14 C13 104.5(8) . . ?
 C14 C15 C16 104.8(8) . . ?
 O1 C16 C15 106.5(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
