#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:26:29 +0300 (Sat, 05 Jun 2021) $
#$Revision: 265871 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/82/7128214.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_7128214
loop_
_publ_author_name
'Kurogi, Takashi'
'Irifune, Keiichi'
'Enoki, Takahiro'
'Takai, Kazuhiko'
_publ_section_title
;
 A trinuclear chromium(iii) chlorocarbyne.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5199
_journal_page_last               5202
_journal_paper_doi               10.1039/d1cc01514a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C25 H48 Cl7 Cr3 O6, 1.5(C5 H12)'
_chemical_formula_sum            'C32.5 H66 Cl7 Cr3 O6'
_chemical_formula_weight         957.00
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-17 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.435(3)
_cell_length_b                   12.435(3)
_cell_length_c                   15.058(4)
_cell_measurement_reflns_used    5613
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     2016.5(9)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16186
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/pentane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 971 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3074
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1207P)²+0.3459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2594
_reflns_number_total             3074
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01514a2.cif
_cod_data_source_block           Cr3CClCl6thf6
_cod_depositor_comments
'Adding full bibliography for 7128214--7128217.cif.'
_cod_original_cell_volume        2016.5(11)
_cod_database_code               7128214
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.819
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'-x, -x+y, z+1/2'
'x-y, -y, 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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1A Cr 0.8827(2) 0.0488(2) 0.56852(11) 0.0211(5) Uani 0.6 1 d . . . A 1
Cr1B Cr 0.9525(3) 0.1189(3) 0.57027(16) 0.0189(6) Uani 0.4 1 d . . . B 2
Cl1B Cl 1.0660(4) 0.2909(4) 0.6574(3) 0.0278(9) Uani 0.4 1 d . . . B 2
Cl1A Cl 1.0528(3) 0.1766(3) 0.66569(17) 0.0232(6) Uani 0.6 1 d . . . A 1
Cl2A Cl 0.7076(3) -0.0671(3) 0.48151(19) 0.0292(7) Uani 0.6 1 d . . . A 1
Cl2B Cl 0.8247(4) -0.0525(4) 0.4738(3) 0.0233(9) Uani 0.4 1 d . . . B 2
C1A C 1.000000 0.000000 0.5119(14) 0.027(5) Uani 0.6 3 d S T P A 1
Cl3A Cl 1.000000 0.000000 0.3925(3) 0.0339(13) Uani 0.6 3 d S T P A 1
C1B C 1.000000 0.000000 0.6287(17) 0.012(5) Uani 0.3999 3 d S T P B 2
Cl3B Cl 1.000000 0.000000 0.7473(4) 0.0261(16) Uani 0.3999 3 d S T P B 2
O1A O 0.9180(10) 0.1997(10) 0.4948(7) 0.028(2) Uani 0.6 1 d D U . A 1
C2A C 0.903(3) 0.2065(16) 0.3976(10) 0.049(3) Uani 0.6 1 d D U . A 1
H2AA H 0.814228 0.158538 0.381121 0.058 Uiso 0.6 1 calc R . . A 1
H2AB H 0.948073 0.171580 0.365275 0.058 Uiso 0.6 1 calc R . . A 1
C3A C 0.9566(19) 0.3431(13) 0.3741(9) 0.063(3) Uani 0.6 1 d D U . A 1
H3AA H 1.036767 0.375173 0.342535 0.076 Uiso 0.6 1 calc R . . A 1
H3AB H 0.898496 0.354384 0.335606 0.076 Uiso 0.6 1 calc R . . A 1
C4A C 0.974(2) 0.4082(14) 0.4594(10) 0.066(3) Uani 0.6 1 d D U . A 1
H4AA H 1.056224 0.485531 0.460288 0.079 Uiso 0.6 1 calc R . . A 1
H4AB H 0.908931 0.430316 0.467775 0.079 Uiso 0.6 1 calc R . . A 1
C5A C 0.9682(14) 0.3261(10) 0.5289(7) 0.036(2) Uani 0.6 1 d D U . A 1
H5AA H 0.914659 0.326228 0.577454 0.043 Uiso 0.6 1 calc R . . A 1
H5AB H 1.052338 0.355761 0.553337 0.043 Uiso 0.6 1 calc R . . A 1
O1B O 0.8911(16) 0.2210(13) 0.4863(10) 0.030(3) Uani 0.4 1 d D U . B 2
C2B C 0.912(4) 0.228(3) 0.3910(11) 0.047(4) Uani 0.4 1 d D U . B 2
H2BA H 0.868706 0.144692 0.363113 0.057 Uiso 0.4 1 calc R . . B 2
H2BB H 1.001722 0.269161 0.376611 0.057 Uiso 0.4 1 calc R . . B 2
C3B C 0.856(3) 0.3055(17) 0.3635(13) 0.059(4) Uani 0.4 1 d D U . B 2
H3BA H 0.879725 0.336656 0.302013 0.071 Uiso 0.4 1 calc R . . B 2
H3BB H 0.764599 0.258857 0.368765 0.071 Uiso 0.4 1 calc R . . B 2
C4B C 0.914(3) 0.4090(15) 0.4300(11) 0.065(4) Uani 0.4 1 d D U . B 2
H4BA H 1.004648 0.462300 0.420820 0.078 Uiso 0.4 1 calc R . . B 2
H4BB H 0.873991 0.460581 0.430359 0.078 Uiso 0.4 1 calc R . . B 2
C5B C 0.884(2) 0.3305(15) 0.5112(11) 0.041(3) Uani 0.4 1 d D U . B 2
H5BA H 0.944880 0.376702 0.558963 0.049 Uiso 0.4 1 calc R . . B 2
H5BB H 0.800101 0.306274 0.532945 0.049 Uiso 0.4 1 calc R . . B 2
O2A O 0.7747(9) 0.1094(10) 0.6562(7) 0.035(2) Uani 0.6 1 d D U . A 1
C6A C 0.6643(11) 0.1109(15) 0.6282(8) 0.044(2) Uani 0.6 1 d D U . A 1
H6AA H 0.599196 0.027118 0.609093 0.053 Uiso 0.6 1 calc R . . A 1
H6AB H 0.683207 0.169468 0.578256 0.053 Uiso 0.6 1 calc R . . A 1
C7A C 0.6224(15) 0.1523(15) 0.7081(8) 0.066(3) Uani 0.6 1 d D U . A 1
H7AA H 0.532047 0.121941 0.708299 0.079 Uiso 0.6 1 calc R . . A 1
H7AB H 0.670029 0.243192 0.717524 0.079 Uiso 0.6 1 calc R . . A 1
C8A C 0.6593(13) 0.0815(15) 0.7703(9) 0.055(3) Uani 0.6 1 d D U . A 1
H8AA H 0.654597 0.105288 0.832313 0.066 Uiso 0.6 1 calc R . . A 1
H8AB H 0.600326 -0.008604 0.763949 0.066 Uiso 0.6 1 calc R . . A 1
C9A C 0.7877(14) 0.107(3) 0.7517(8) 0.043(3) Uani 0.6 1 d D U . A 1
H9AA H 0.852549 0.187529 0.776003 0.052 Uiso 0.6 1 calc R . . A 1
H9AB H 0.801882 0.039201 0.771681 0.052 Uiso 0.6 1 calc R . . A 1
O2B O 0.7897(14) 0.0783(15) 0.6473(11) 0.032(3) Uani 0.4 1 d D U . B 2
C6B C 0.6685(14) 0.030(2) 0.6072(11) 0.038(3) Uani 0.4 1 d D U . B 2
H6BA H 0.632338 -0.058656 0.591876 0.045 Uiso 0.4 1 calc R . . B 2
H6BB H 0.673466 0.077164 0.552792 0.045 Uiso 0.4 1 calc R . . B 2
C7B C 0.5929(19) 0.048(2) 0.6775(11) 0.051(3) Uani 0.4 1 d D U . B 2
H7BA H 0.502651 -0.005785 0.667083 0.061 Uiso 0.4 1 calc R . . B 2
H7BB H 0.613831 0.135352 0.682464 0.061 Uiso 0.4 1 calc R . . B 2
C8B C 0.6358(18) 0.006(2) 0.7573(13) 0.055(4) Uani 0.4 1 d D U . B 2
H8BA H 0.605727 0.021508 0.814102 0.066 Uiso 0.4 1 calc R . . B 2
H8BB H 0.615606 -0.081419 0.753435 0.066 Uiso 0.4 1 calc R . . B 2
C9B C 0.7701(19) 0.097(3) 0.7400(13) 0.042(4) Uani 0.4 1 d D U . B 2
H9BA H 0.788427 0.182977 0.750249 0.050 Uiso 0.4 1 calc R . . B 2
H9BB H 0.823820 0.079849 0.779207 0.050 Uiso 0.4 1 calc R . . B 2
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1A Cr1A Cl1A 89.71(14) 2_645 . ?
Cl2A Cr1A Cl1A 90.89(14) . 2_645 ?
Cl2A Cr1A Cl1A 174.52(13) . . ?
C1A Cr1A Cl1A 85.8(4) . . ?
C1A Cr1A Cl1A 86.2(4) . 2_645 ?
C1A Cr1A Cl2A 99.7(4) . . ?
C1A Cr1A O1A 101.0(5) . . ?
C1A Cr1A O2A 168.6(5) . . ?
O1A Cr1A Cl1A 172.8(3) . 2_645 ?
O1A Cr1A Cl1A 90.6(3) . . ?
O1A Cr1A Cl2A 88.1(3) . . ?
O1A Cr1A O2A 84.4(4) . . ?
O2A Cr1A Cl1A 88.5(3) . 2_645 ?
O2A Cr1A Cl1A 84.1(3) . . ?
O2A Cr1A Cl2A 90.4(3) . . ?
Cl1B Cr1B Cl2B 175.1(2) . . ?
Cl1B Cr1B Cl2B 91.9(2) . 3_765 ?
Cl2B Cr1B Cl2B 89.4(2) 3_765 . ?
C1B Cr1B Cl1B 99.4(5) . . ?
C1B Cr1B Cl2B 86.5(5) . 3_765 ?
C1B Cr1B Cl2B 85.5(5) . . ?
C1B Cr1B O1B 169.0(7) . . ?
C1B Cr1B O2B 100.1(6) . . ?
O1B Cr1B Cl1B 91.1(4) . . ?
O1B Cr1B Cl2B 89.6(4) . 3_765 ?
O1B Cr1B Cl2B 84.1(4) . . ?
O2B Cr1B Cl1B 88.8(4) . . ?
O2B Cr1B Cl2B 89.4(4) . . ?
O2B Cr1B Cl2B 173.1(4) . 3_765 ?
O2B Cr1B O1B 83.5(6) . . ?
Cr1A Cl1A Cr1A 83.31(12) 3_765 . ?
Cr1B Cl2B Cr1B 84.07(18) 2_645 . ?
Cr1A C1A Cr1A 103.6(6) . 2_645 ?
Cr1A C1A Cr1A 103.6(6) 3_765 2_645 ?
Cr1A C1A Cr1A 103.6(6) . 3_765 ?
Cl3A C1A Cr1A 114.9(5) . 2_645 ?
Cl3A C1A Cr1A 114.9(5) . 3_765 ?
Cl3A C1A Cr1A 114.9(5) . . ?
Cr1B C1B Cr1B 102.8(8) 2_645 . ?
Cr1B C1B Cr1B 102.8(8) 3_765 . ?
Cl3B C1B Cr1B 115.5(6) . . ?
Cl3B C1B Cr1B 115.5(6) . 2_645 ?
C2A O1A Cr1A 128.1(9) . . ?
C5A O1A Cr1A 125.4(7) . . ?
C5A O1A C2A 106.4(10) . . ?
O1A C2A C3A 107.2(12) . . ?
C4A C3A C2A 105.8(12) . . ?
C5A C4A C3A 107.7(12) . . ?
C4A C5A O1A 110.5(10) . . ?
C2B O1B Cr1B 120.1(12) . . ?
C5B O1B Cr1B 126.6(12) . . ?
C5B O1B C2B 107.0(13) . . ?
O1B C2B C3B 100.5(15) . . ?
C4B C3B C2B 100.9(16) . . ?
C5B C4B C3B 97.5(13) . . ?
O1B C5B C4B 106.8(13) . . ?
C6A O2A Cr1A 124.1(8) . . ?
C6A O2A C9A 114.0(11) . . ?
C9A O2A Cr1A 118.7(10) . . ?
O2A C6A C7A 105.4(10) . . ?
C6A C7A C8A 92.2(10) . . ?
C9A C8A C7A 111.5(14) . . ?
O2A C9A C8A 94.1(10) . . ?
C6B O2B Cr1B 122.2(11) . . ?
C6B O2B C9B 104.1(15) . . ?
C9B O2B Cr1B 133.5(12) . . ?
O2B C6B C7B 104.2(14) . . ?
C6B C7B C8B 99.1(15) . . ?
C9B C8B C7B 93.3(18) . . ?
O2B C9B C8B 105.0(17) . . ?
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
Cr1A Cl1A 2.389(3) 2_645 ?
Cr1A Cl1A 2.404(3) . ?
Cr1A Cl2A 2.323(4) . ?
Cr1A C1A 2.027(9) . ?
Cr1A O1A 2.030(11) . ?
Cr1A O2A 2.264(11) . ?
Cr1B Cl1B 2.295(5) . ?
Cr1B Cl2B 2.407(5) . ?
Cr1B Cl2B 2.367(5) 3_765 ?
Cr1B C1B 2.044(11) . ?
Cr1B O1B 2.183(14) . ?
Cr1B O2B 2.163(17) . ?
C1A Cl3A 1.80(2) . ?
C1B Cl3B 1.79(3) . ?
O1A C2A 1.483(15) . ?
O1A C5A 1.464(13) . ?
C2A C3A 1.524(19) . ?
C3A C4A 1.475(17) . ?
C4A C5A 1.437(16) . ?
O1B C2B 1.454(7) . ?
O1B C5B 1.454(7) . ?
C2B C3B 1.502(7) . ?
C3B C4B 1.499(7) . ?
C4B C5B 1.492(7) . ?
O2A C6A 1.445(7) . ?
O2A C9A 1.449(7) . ?
C6A C7A 1.500(7) . ?
C7A C8A 1.506(7) . ?
C8A C9A 1.491(7) . ?
O2B C6B 1.446(7) . ?
O2B C9B 1.456(7) . ?
C6B C7B 1.501(7) . ?
C7B C8B 1.505(8) . ?
C8B C9B 1.498(8) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1A O1A C2A C3A -173.4(11) . . . . ?
Cr1A O1A C5A C4A -176.6(11) . . . . ?
Cr1A O2A C6A C7A 177.9(9) . . . . ?
Cr1A O2A C9A C8A -149.7(11) . . . . ?
Cr1B O1B C2B C3B -179.7(14) . . . . ?
Cr1B O1B C5B C4B 146.2(15) . . . . ?
Cr1B O2B C6B C7B -165.6(13) . . . . ?
Cr1B O2B C9B C8B -158.5(15) . . . . ?
O1A C2A C3A C4A -13(3) . . . . ?
C2A O1A C5A C4A 5.2(18) . . . . ?
C2A C3A C4A C5A 16(2) . . . . ?
C3A C4A C5A O1A -13(2) . . . . ?
C5A O1A C2A C3A 5(2) . . . . ?
O1B C2B C3B C4B 48(2) . . . . ?
C2B O1B C5B C4B -5(3) . . . . ?
C2B C3B C4B C5B -50(2) . . . . ?
C3B C4B C5B O1B 34(3) . . . . ?
C5B O1B C2B C3B -26(3) . . . . ?
O2A C6A C7A C8A -37.1(14) . . . . ?
C6A O2A C9A C8A 11(2) . . . . ?
C6A C7A C8A C9A 48.9(17) . . . . ?
C7A C8A C9A O2A -39(2) . . . . ?
C9A O2A C6A C7A 18.6(19) . . . . ?
O2B C6B C7B C8B -43(2) . . . . ?
C6B O2B C9B C8B 26(3) . . . . ?
C6B C7B C8B C9B 55(2) . . . . ?
C7B C8B C9B O2B -51(3) . . . . ?
C9B O2B C6B C7B 10(2) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.85(8)
2 0.15(8)
