#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:36:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179979 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/73/7027354.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027354
loop_
_publ_author_name
'Chew, Kong Chin'
'Clegg, William'
'Coles, Martyn P.'
'Elsegood, Mark R. J.'
'Gibson, Vernon C.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Synthesis and characterisation of 2,6-diisopropylphenylimido complexes of
 chromium in oxidation states IV--VI
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2633
_journal_paper_doi               10.1039/a901790i
_journal_year                    1999
_chemical_formula_sum            'C36 H52 Cl Cr N3'
_chemical_formula_weight         614.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom except h1 coords refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'all non-H found by direct methods'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.707(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4714(11)
_cell_length_b                   15.411(2)
_cell_length_c                   21.493(2)
_cell_measurement_reflns_used    8295
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.10
_cell_volume                     3456.7(7)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14712
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.203
_refine_ls_goodness_of_fit_obs   1.232
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.232
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_obs          0.0588
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+5.2883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1248
_refine_ls_wR_factor_obs         0.1177
_reflns_number_observed          4943
_reflns_number_total             5734
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901790isup1.cif
_cod_data_source_block           vcg72
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+5.2883P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+5.2883P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3456.7(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027354
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cr1 Cr 0.41883(5) 0.37978(3) 0.20426(2) 0.0229(2) Uani 1 d .
Cl1 Cl 0.53647(8) 0.49279(6) 0.17842(4) 0.0356(2) Uani 1 d .
N1 N 0.2692(3) 0.4121(2) 0.23745(13) 0.0273(7) Uani 1 d .
H1 H 0.2827(36) 0.4115(26) 0.2724(18) 0.041 Uiso 1 d .
C1 C 0.1369(3) 0.4098(2) 0.2172(2) 0.0282(7) Uani 1 d .
C2 C 0.0925(3) 0.4505(2) 0.1611(2) 0.0320(8) Uani 1 d .
C3 C -0.0393(3) 0.4488(3) 0.1441(2) 0.0404(9) Uani 1 d .
H3 H -0.0719(3) 0.4757(3) 0.1064(2) 0.048 Uiso 1 calc R
C4 C -0.1230(3) 0.4084(3) 0.1815(2) 0.0440(10) Uani 1 d .
H4 H -0.2123(3) 0.4080(3) 0.1693(2) 0.053 Uiso 1 calc R
C5 C -0.0774(3) 0.3688(3) 0.2362(2) 0.0425(10) Uani 1 d .
H5 H -0.1361(3) 0.3412(3) 0.2612(2) 0.051 Uiso 1 calc R
C6 C 0.0528(3) 0.3681(2) 0.2558(2) 0.0338(8) Uani 1 d .
C7 C 0.1788(3) 0.5009(3) 0.1205(2) 0.0380(9) Uani 1 d .
H7 H 0.2688(3) 0.4946(3) 0.1393(2) 0.046 Uiso 1 calc R
C8 C 0.1457(4) 0.5972(3) 0.1200(2) 0.0634(13) Uani 1 d .
H8A H 0.2042(19) 0.6287(4) 0.0946(12) 0.095 Uiso 1 calc R
H8B H 0.1544(29) 0.6197(5) 0.1628(3) 0.095 Uiso 1 calc R
H8C H 0.0573(11) 0.6053(3) 0.1022(13) 0.095 Uiso 1 calc R
C9 C 0.1733(4) 0.4645(3) 0.0543(2) 0.0568(12) Uani 1 d .
H9A H 0.2296(23) 0.4986(12) 0.0294(4) 0.085 Uiso 1 calc R
H9B H 0.0852(7) 0.4676(18) 0.0353(5) 0.085 Uiso 1 calc R
H9C H 0.2018(27) 0.4039(7) 0.0558(2) 0.085 Uiso 1 calc R
C10 C 0.1028(4) 0.3254(3) 0.3170(2) 0.0397(9) Uani 1 d .
H10 H 0.1888(4) 0.3003(3) 0.3105(2) 0.048 Uiso 1 calc R
C11 C 0.1224(4) 0.3945(3) 0.3688(2) 0.0533(11) Uani 1 d .
H11A H 0.1672(24) 0.3684(5) 0.4060(5) 0.080 Uiso 1 calc R
H11B H 0.0389(4) 0.4165(13) 0.3790(9) 0.080 Uiso 1 calc R
H11C H 0.1737(23) 0.4424(9) 0.3542(5) 0.080 Uiso 1 calc R
C12 C 0.0202(4) 0.2523(3) 0.3388(2) 0.0631(13) Uani 1 d .
H12A H 0.0656(13) 0.2229(13) 0.3745(9) 0.095 Uiso 1 calc R
H12B H 0.0025(25) 0.2107(11) 0.3047(5) 0.095 Uiso 1 calc R
H12C H -0.0606(13) 0.2761(4) 0.3512(14) 0.095 Uiso 1 calc R
N2 N 0.5044(2) 0.3298(2) 0.26145(12) 0.0271(6) Uani 1 d .
C13 C 0.5746(3) 0.2785(2) 0.30477(15) 0.0273(7) Uani 1 d .
C14 C 0.6362(3) 0.2026(2) 0.2862(2) 0.0301(8) Uani 1 d .
C15 C 0.7050(3) 0.1540(2) 0.3324(2) 0.0366(9) Uani 1 d .
H15 H 0.7470(3) 0.1023(2) 0.3211(2) 0.044 Uiso 1 calc R
C16 C 0.7131(3) 0.1796(3) 0.3939(2) 0.0402(9) Uani 1 d .
H16 H 0.7604(3) 0.1454(3) 0.4245(2) 0.048 Uiso 1 calc R
C17 C 0.6538(3) 0.2539(3) 0.4116(2) 0.0407(9) Uani 1 d .
H17 H 0.6611(3) 0.2706(3) 0.4543(2) 0.049 Uiso 1 calc R
C18 C 0.5829(3) 0.3053(2) 0.3680(2) 0.0325(8) Uani 1 d .
C19 C 0.6251(3) 0.1731(2) 0.2186(2) 0.0325(8) Uani 1 d .
H19 H 0.5917(3) 0.2230(2) 0.1923(2) 0.039 Uiso 1 calc R
C20 C 0.7535(4) 0.1468(4) 0.1965(2) 0.0688(15) Uani 1 d .
H20A H 0.8141(10) 0.1951(8) 0.2029(15) 0.103 Uiso 1 calc R
H20B H 0.7427(7) 0.1322(22) 0.1520(4) 0.103 Uiso 1 calc R
H20C H 0.7866(16) 0.0962(14) 0.2202(11) 0.103 Uiso 1 calc R
C21 C 0.5310(5) 0.1004(3) 0.2096(2) 0.074(2) Uani 1 d .
H21A H 0.4488(11) 0.1183(8) 0.2243(15) 0.110 Uiso 1 calc R
H21B H 0.5635(16) 0.0497(8) 0.2335(13) 0.110 Uiso 1 calc R
H21C H 0.5188(26) 0.0854(16) 0.1652(3) 0.110 Uiso 1 calc R
C22 C 0.5223(4) 0.3894(3) 0.3866(2) 0.0440(10) Uani 1 d .
H22 H 0.4504(4) 0.4030(3) 0.3546(2) 0.053 Uiso 1 calc R
C23 C 0.4674(5) 0.3844(4) 0.4497(2) 0.076(2) Uani 1 d .
H23A H 0.4227(30) 0.4387(10) 0.4576(8) 0.114 Uiso 1 calc R
H23B H 0.5370(6) 0.3754(24) 0.4824(3) 0.114 Uiso 1 calc R
H23C H 0.4070(26) 0.3359(15) 0.4498(6) 0.114 Uiso 1 calc R
C24 C 0.6199(5) 0.4617(3) 0.3855(3) 0.079(2) Uani 1 d .
H24A H 0.5821(13) 0.5159(6) 0.3992(17) 0.119 Uiso 1 calc R
H24B H 0.6453(27) 0.4688(16) 0.3429(4) 0.119 Uiso 1 calc R
H24C H 0.6953(16) 0.4472(11) 0.4136(13) 0.119 Uiso 1 calc R
N3 N 0.3825(2) 0.3193(2) 0.14157(12) 0.0245(6) Uani 1 d .
C25 C 0.3830(3) 0.2466(2) 0.10344(14) 0.0254(7) Uani 1 d .
C26 C 0.2850(3) 0.1844(2) 0.10570(15) 0.0289(8) Uani 1 d .
C27 C 0.2893(3) 0.1122(2) 0.0670(2) 0.0352(8) Uani 1 d .
H27 H 0.2236(3) 0.0697(2) 0.0674(2) 0.042 Uiso 1 calc R
C28 C 0.3863(3) 0.1006(3) 0.0279(2) 0.0396(9) Uani 1 d .
H28 H 0.3878(3) 0.0505(3) 0.0022(2) 0.048 Uiso 1 calc R
C29 C 0.4821(3) 0.1634(3) 0.0267(2) 0.0377(9) Uani 1 d .
H29 H 0.5483(3) 0.1554(3) -0.0005(2) 0.045 Uiso 1 calc R
C30 C 0.4839(3) 0.2369(2) 0.0636(2) 0.0315(8) Uani 1 d .
C31 C 0.1774(3) 0.1963(2) 0.1480(2) 0.0349(8) Uani 1 d .
H31 H 0.2022(3) 0.2448(2) 0.1776(2) 0.042 Uiso 1 calc R
C32 C 0.1545(4) 0.1151(3) 0.1870(2) 0.0546(11) Uani 1 d .
H32A H 0.0859(19) 0.1266(7) 0.2143(10) 0.082 Uiso 1 calc R
H32B H 0.2333(9) 0.1002(11) 0.2125(10) 0.082 Uiso 1 calc R
H32C H 0.1296(26) 0.0666(6) 0.1591(2) 0.082 Uiso 1 calc R
C33 C 0.0543(3) 0.2225(3) 0.1103(2) 0.0488(11) Uani 1 d .
H33A H -0.0115(9) 0.2362(17) 0.1387(2) 0.073 Uiso 1 calc R
H33B H 0.0246(14) 0.1745(7) 0.0829(9) 0.073 Uiso 1 calc R
H33C H 0.0703(7) 0.2736(11) 0.0849(10) 0.073 Uiso 1 calc R
C34 C 0.5846(3) 0.3069(2) 0.0611(2) 0.0348(8) Uani 1 d .
H34 H 0.6064(3) 0.3271(2) 0.1049(2) 0.042 Uiso 1 calc R
C35 C 0.7093(3) 0.2763(3) 0.0358(2) 0.0469(10) Uani 1 d .
H35A H 0.7735(9) 0.3226(7) 0.0409(12) 0.070 Uiso 1 calc R
H35B H 0.6933(7) 0.2621(17) -0.0086(4) 0.070 Uiso 1 calc R
H35C H 0.7409(14) 0.2247(11) 0.0588(9) 0.070 Uiso 1 calc R
C36 C 0.5313(4) 0.3852(3) 0.0239(2) 0.0486(10) Uani 1 d .
H36A H 0.5966(10) 0.4308(7) 0.0246(11) 0.073 Uiso 1 calc R
H36B H 0.4554(16) 0.4073(11) 0.0425(8) 0.073 Uiso 1 calc R
H36C H 0.5077(24) 0.3677(5) -0.0194(4) 0.073 Uiso 1 calc R
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'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2 Cr1 N3 114.69(13)
N2 Cr1 N1 105.34(13)
N3 Cr1 N1 108.73(12)
N2 Cr1 Cl1 105.80(10)
N3 Cr1 Cl1 109.37(9)
N1 Cr1 Cl1 112.94(10)
C1 N1 Cr1 135.6(2)
C2 C1 C6 121.9(3)
C2 C1 N1 119.9(3)
C6 C1 N1 118.1(3)
C3 C2 C1 117.8(3)
C3 C2 C7 118.7(3)
C1 C2 C7 123.4(3)
C4 C3 C2 121.0(4)
C5 C4 C3 120.3(3)
C4 C5 C6 121.7(3)
C5 C6 C1 117.4(3)
C5 C6 C10 121.6(3)
C1 C6 C10 121.1(3)
C2 C7 C8 110.9(3)
C2 C7 C9 111.6(3)
C8 C7 C9 111.1(3)
C12 C10 C6 115.0(3)
C12 C10 C11 109.6(3)
C6 C10 C11 109.9(3)
C13 N2 Cr1 172.7(2)
N2 C13 C14 120.9(3)
N2 C13 C18 117.7(3)
C14 C13 C18 121.3(3)
C15 C14 C13 117.8(3)
C15 C14 C19 121.0(3)
C13 C14 C19 121.2(3)
C16 C15 C14 121.1(4)
C17 C16 C15 120.8(3)
C16 C17 C18 121.1(4)
C17 C18 C13 117.8(3)
C17 C18 C22 121.4(3)
C13 C18 C22 120.7(3)
C21 C19 C20 110.6(4)
C21 C19 C14 110.2(3)
C20 C19 C14 112.3(3)
C18 C22 C24 109.2(3)
C18 C22 C23 113.1(3)
C24 C22 C23 111.0(4)
C25 N3 Cr1 157.3(2)
N3 C25 C26 119.4(3)
N3 C25 C30 118.6(3)
C26 C25 C30 122.0(3)
C27 C26 C25 117.7(3)
C27 C26 C31 121.2(3)
C25 C26 C31 121.2(3)
C28 C27 C26 121.8(3)
C27 C28 C29 119.1(3)
C30 C29 C28 122.3(3)
C29 C30 C25 117.1(3)
C29 C30 C34 122.8(3)
C25 C30 C34 120.1(3)
C26 C31 C33 110.6(3)
C26 C31 C32 112.7(3)
C33 C31 C32 110.1(3)
C30 C34 C36 110.8(3)
C30 C34 C35 114.2(3)
C36 C34 C35 110.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cr1 N2 1.651(3)
Cr1 N3 1.657(3)
Cr1 N1 1.843(3)
Cr1 Cl1 2.2297(10)
N1 C1 1.418(4)
C1 C2 1.404(5)
C1 C6 1.414(5)
C2 C3 1.399(5)
C2 C7 1.520(5)
C3 C4 1.385(5)
C4 C5 1.374(5)
C5 C6 1.393(5)
C6 C10 1.523(5)
C7 C8 1.524(6)
C7 C9 1.526(5)
C10 C12 1.518(5)
C10 C11 1.542(5)
N2 C13 1.386(4)
C13 C14 1.410(5)
C13 C18 1.415(5)
C14 C15 1.395(5)
C14 C19 1.518(5)
C15 C16 1.375(5)
C16 C17 1.371(5)
C17 C18 1.394(5)
C18 C22 1.511(5)
C19 C21 1.495(5)
C19 C20 1.518(5)
C22 C24 1.513(6)
C22 C23 1.516(6)
N3 C25 1.388(4)
C25 C26 1.408(4)
C25 C30 1.422(4)
C26 C27 1.393(5)
C26 C31 1.516(5)
C27 C28 1.382(5)
C28 C29 1.396(5)
C29 C30 1.382(5)
C30 C34 1.513(5)
C31 C33 1.521(5)
C31 C32 1.537(5)
C34 C36 1.527(5)
C34 C35 1.530(5)
