#------------------------------------------------------------------------------
#$Date: 2022-11-15 02:10:49 +0200 (Tue, 15 Nov 2022) $
#$Revision: 279275 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/17/7711756.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_7711756
loop_
_publ_author_name
'Luz, Christian'
'Glok, Eduard'
'Horrer, Günther'
'Radius, Udo'
_publ_section_title
;
 N Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Complexes of
 Molybdenum(IV) and Tungsten(IV)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03409C
_journal_year                    2022
_chemical_formula_moiety         'C22 H40 Cl4 N4 W, 4(C H Cl3)'
_chemical_formula_sum            'C26 H44 Cl16 N4 W'
_chemical_formula_weight         1163.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-10-20 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                116.175(2)
_cell_angle_beta                 98.184(2)
_cell_angle_gamma                95.091(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1142(2)
_cell_length_b                   11.0375(2)
_cell_length_c                   12.2193(3)
_cell_measurement_reflns_used    16490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.4990
_cell_measurement_theta_min      4.1170
_cell_volume                     1075.94(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         80.227
_diffrn_reflns_theta_min         4.117
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    14.331
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.73a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0299P)²+1.2208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4529
_reflns_number_total             4589
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03409c2.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        1075.94(4)
_cod_database_code               7711756
_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_min   0.124
_shelx_estimated_absorpt_t_max   0.222
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
W001 W 0.500000 0.500000 0.000000 0.01204(6) Uani 1 2 d S . P . .
Cl02 Cl 0.60987(7) 0.73486(6) 0.09240(5) 0.01678(12) Uani 1 1 d . . . . .
Cl03 Cl 0.67911(6) 0.48569(6) 0.15212(5) 0.01587(12) Uani 1 1 d . . . . .
Cl04 Cl 0.49451(8) 1.19382(8) 0.53881(7) 0.02931(15) Uani 1 1 d . . . . .
Cl05 Cl 0.08324(8) 0.95540(8) 0.81374(7) 0.03032(16) Uani 1 1 d . . . . .
Cl06 Cl 0.20117(8) 1.26013(8) 0.48731(7) 0.02869(16) Uani 1 1 d . . . . .
Cl07 Cl 0.22909(9) 1.04327(7) 0.55620(7) 0.02824(15) Uani 1 1 d . . . . .
Cl08 Cl 0.20968(8) 0.76062(8) 0.61831(7) 0.02867(15) Uani 1 1 d . . . . .
Cl09 Cl 0.36438(9) 0.87553(8) 0.87595(7) 0.03110(16) Uani 1 1 d . . . . .
N00A N 0.2883(2) 0.4812(2) 0.19256(19) 0.0140(4) Uani 1 1 d . . . . .
N00B N 0.2432(2) 0.6493(2) 0.15396(19) 0.0140(4) Uani 1 1 d . . . . .
C00C C 0.0302(3) 0.7308(3) 0.2724(3) 0.0208(5) Uani 1 1 d . . . . .
H00A H -0.061076 0.695529 0.207097 0.031 Uiso 1 1 calc R U . . .
H00B H 0.070013 0.824461 0.290073 0.031 Uiso 1 1 calc R U . . .
H00C H 0.006229 0.731065 0.348161 0.031 Uiso 1 1 calc R U . . .
C00D C 0.1460(3) 0.6411(3) 0.2294(2) 0.0158(5) Uani 1 1 d . . . . .
C00E C 0.3605(3) 0.3706(3) 0.2032(2) 0.0159(5) Uani 1 1 d . . . . .
H00E H 0.435556 0.350406 0.147879 0.019 Uiso 1 1 calc R U . . .
C00F C 0.3325(3) 0.5502(3) 0.1297(2) 0.0132(5) Uani 1 1 d . . . . .
C00G C 0.2479(3) 0.7508(3) 0.1054(2) 0.0166(5) Uani 1 1 d . . . . .
H00G H 0.321248 0.727070 0.048591 0.020 Uiso 1 1 calc R U . . .
C00H C 0.4493(3) 0.4192(3) 0.3351(2) 0.0197(5) Uani 1 1 d . . . . .
H00D H 0.500388 0.346059 0.338477 0.030 Uiso 1 1 calc R U . . .
H00F H 0.380425 0.442389 0.393289 0.030 Uiso 1 1 calc R U . . .
H00H H 0.524153 0.500312 0.358229 0.030 Uiso 1 1 calc R U . . .
C00I C 0.1731(3) 0.5358(3) 0.2533(2) 0.0166(5) Uani 1 1 d . . . . .
C00J C 0.0901(3) 0.4810(3) 0.3236(3) 0.0210(5) Uani 1 1 d . . . . .
H00I H 0.030361 0.390833 0.265662 0.032 Uiso 1 1 calc R U . . .
H00J H 0.023304 0.543832 0.364884 0.032 Uiso 1 1 calc R U . . .
H00K H 0.162321 0.472348 0.386254 0.032 Uiso 1 1 calc R U . . .
C00K C 0.2494(3) 0.2377(3) 0.1548(3) 0.0198(5) Uani 1 1 d . . . . .
H00L H 0.186042 0.218877 0.075297 0.030 Uiso 1 1 calc R U . . .
H00M H 0.185867 0.246708 0.215373 0.030 Uiso 1 1 calc R U . . .
H00N H 0.304763 0.162024 0.142500 0.030 Uiso 1 1 calc R U . . .
C00L C 0.3101(3) 0.8966(3) 0.2092(3) 0.0213(5) Uani 1 1 d . . . . .
H00O H 0.335338 0.956495 0.172264 0.032 Uiso 1 1 calc R U . . .
H00P H 0.400596 0.895590 0.262545 0.032 Uiso 1 1 calc R U . . .
H00Q H 0.233942 0.930812 0.259186 0.032 Uiso 1 1 calc R U . . .
C00M C 0.0974(3) 0.7375(3) 0.0259(3) 0.0230(6) Uani 1 1 d . . . . .
H00R H 0.108662 0.793959 -0.016709 0.035 Uiso 1 1 calc R U . . .
H00S H 0.023616 0.768479 0.079113 0.035 Uiso 1 1 calc R U . . .
H00T H 0.062679 0.641476 -0.035958 0.035 Uiso 1 1 calc R U . . .
C00N C 0.2508(3) 0.9070(3) 0.7654(3) 0.0231(6) Uani 1 1 d . . . . .
H1A H 0.300(4) 0.976(4) 0.760(3) 0.017(8) Uiso 1 1 d . . . . .
C00O C 0.3163(3) 1.2040(3) 0.5785(3) 0.0208(5) Uani 1 1 d . . . . .
H1 H 0.332(3) 1.269(3) 0.662(3) 0.011(7) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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
C00F W001 C00F 180.0 2_665 . ?
C00F W001 Cl03 90.46(6) 2_665 2_665 ?
C00F W001 Cl03 89.54(6) . 2_665 ?
C00F W001 Cl03 89.54(6) 2_665 . ?
C00F W001 Cl03 90.46(6) . . ?
Cl03 W001 Cl03 180.00(3) 2_665 . ?
C00F W001 Cl02 89.25(6) 2_665 . ?
C00F W001 Cl02 90.75(6) . . ?
Cl03 W001 Cl02 93.97(2) 2_665 . ?
Cl03 W001 Cl02 86.03(2) . . ?
C00F W001 Cl02 90.75(6) 2_665 2_665 ?
C00F W001 Cl02 89.25(6) . 2_665 ?
Cl03 W001 Cl02 86.03(2) 2_665 2_665 ?
Cl03 W001 Cl02 93.97(2) . 2_665 ?
Cl02 W001 Cl02 180.0 . 2_665 ?
C00F N00A C00I 111.0(2) . . ?
C00F N00A C00E 124.7(2) . . ?
C00I N00A C00E 124.1(2) . . ?
C00F N00B C00D 111.1(2) . . ?
C00F N00B C00G 124.8(2) . . ?
C00D N00B C00G 124.1(2) . . ?
C00D C00C H00A 109.5 . . ?
C00D C00C H00B 109.5 . . ?
H00A C00C H00B 109.5 . . ?
C00D C00C H00C 109.5 . . ?
H00A C00C H00C 109.5 . . ?
H00B C00C H00C 109.5 . . ?
C00I C00D N00B 107.1(2) . . ?
C00I C00D C00C 127.0(2) . . ?
N00B C00D C00C 125.9(2) . . ?
N00A C00E C00K 112.4(2) . . ?
N00A C00E C00H 111.1(2) . . ?
C00K C00E C00H 113.4(2) . . ?
N00A C00E H00E 106.5 . . ?
C00K C00E H00E 106.5 . . ?
C00H C00E H00E 106.5 . . ?
N00A C00F N00B 104.1(2) . . ?
N00A C00F W001 128.04(18) . . ?
N00B C00F W001 127.69(17) . . ?
N00B C00G C00M 111.4(2) . . ?
N00B C00G C00L 111.9(2) . . ?
C00M C00G C00L 113.9(2) . . ?
N00B C00G H00G 106.3 . . ?
C00M C00G H00G 106.3 . . ?
C00L C00G H00G 106.3 . . ?
C00E C00H H00D 109.5 . . ?
C00E C00H H00F 109.5 . . ?
H00D C00H H00F 109.5 . . ?
C00E C00H H00H 109.5 . . ?
H00D C00H H00H 109.5 . . ?
H00F C00H H00H 109.5 . . ?
C00D C00I N00A 106.7(2) . . ?
C00D C00I C00J 127.2(2) . . ?
N00A C00I C00J 126.0(2) . . ?
C00I C00J H00I 109.5 . . ?
C00I C00J H00J 109.5 . . ?
H00I C00J H00J 109.5 . . ?
C00I C00J H00K 109.5 . . ?
H00I C00J H00K 109.5 . . ?
H00J C00J H00K 109.5 . . ?
C00E C00K H00L 109.5 . . ?
C00E C00K H00M 109.5 . . ?
H00L C00K H00M 109.5 . . ?
C00E C00K H00N 109.5 . . ?
H00L C00K H00N 109.5 . . ?
H00M C00K H00N 109.5 . . ?
C00G C00L H00O 109.5 . . ?
C00G C00L H00P 109.5 . . ?
H00O C00L H00P 109.5 . . ?
C00G C00L H00Q 109.5 . . ?
H00O C00L H00Q 109.5 . . ?
H00P C00L H00Q 109.5 . . ?
C00G C00M H00R 109.5 . . ?
C00G C00M H00S 109.5 . . ?
H00R C00M H00S 109.5 . . ?
C00G C00M H00T 109.5 . . ?
H00R C00M H00T 109.5 . . ?
H00S C00M H00T 109.5 . . ?
Cl05 C00N Cl09 110.58(16) . . ?
Cl05 C00N Cl08 110.14(16) . . ?
Cl09 C00N Cl08 110.58(17) . . ?
Cl05 C00N H1A 108(2) . . ?
Cl09 C00N H1A 108(2) . . ?
Cl08 C00N H1A 109(2) . . ?
Cl04 C00O Cl07 110.68(16) . . ?
Cl04 C00O Cl06 110.19(16) . . ?
Cl07 C00O Cl06 109.63(16) . . ?
Cl04 C00O H1 106.7(19) . . ?
Cl07 C00O H1 111.0(19) . . ?
Cl06 C00O H1 108.6(19) . . ?
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
W001 C00F 2.283(2) 2_665 ?
W001 C00F 2.283(2) . ?
W001 Cl03 2.3635(6) 2_665 ?
W001 Cl03 2.3635(6) . ?
W001 Cl02 2.3733(6) . ?
W001 Cl02 2.3734(6) 2_665 ?
Cl04 C00O 1.759(3) . ?
Cl05 C00N 1.757(3) . ?
Cl06 C00O 1.766(3) . ?
Cl07 C00O 1.765(3) . ?
Cl08 C00N 1.767(3) . ?
Cl09 C00N 1.760(3) . ?
N00A C00F 1.372(3) . ?
N00A C00I 1.399(3) . ?
N00A C00E 1.483(3) . ?
N00B C00F 1.374(3) . ?
N00B C00D 1.391(3) . ?
N00B C00G 1.481(3) . ?
C00C C00D 1.501(4) . ?
C00C H00A 0.9800 . ?
C00C H00B 0.9800 . ?
C00C H00C 0.9800 . ?
C00D C00I 1.353(4) . ?
C00E C00K 1.526(4) . ?
C00E C00H 1.526(4) . ?
C00E H00E 1.0000 . ?
C00G C00M 1.519(4) . ?
C00G C00L 1.533(4) . ?
C00G H00G 1.0000 . ?
C00H H00D 0.9800 . ?
C00H H00F 0.9800 . ?
C00H H00H 0.9800 . ?
C00I C00J 1.496(4) . ?
C00J H00I 0.9800 . ?
C00J H00J 0.9800 . ?
C00J H00K 0.9800 . ?
C00K H00L 0.9800 . ?
C00K H00M 0.9800 . ?
C00K H00N 0.9800 . ?
C00L H00O 0.9800 . ?
C00L H00P 0.9800 . ?
C00L H00Q 0.9800 . ?
C00M H00R 0.9800 . ?
C00M H00S 0.9800 . ?
C00M H00T 0.9800 . ?
C00N H1A 0.88(4) . ?
C00O H1 0.93(3) . ?
