#------------------------------------------------------------------------------
#$Date: 2020-03-05 02:09:08 +0200 (Thu, 05 Mar 2020) $
#$Revision: 248945 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/32/7703297.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_7703297
loop_
_publ_author_name
'Noor, Awal'
'Qayyum, Sadaf'
'Schwarz, Stefan'
'Dietel, Thomas'
'Kempe, Rhett'
_publ_section_title
;
 Formation of a dimeric tungsten(i) complex via C-H activation.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1992
_journal_page_last               1996
_journal_paper_doi               10.1039/c9dt04847b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C64 H86 Cl4 N4 W2'
_chemical_formula_weight         1420.87
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-10-22 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.866(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.9780(9)
_cell_length_b                   26.9280(9)
_cell_length_c                   11.7290(5)
_cell_measurement_reflns_used    11835
_cell_measurement_temperature    133(2)
_cell_volume                     7851.9(5)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_sigmaI/netI    0.2108
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24750
_diffrn_reflns_theta_full        24.61
_diffrn_reflns_theta_max         24.61
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    3.096
_exptl_absorpt_correction_T_max  0.8082
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.706
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.706
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0411P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                3021
_reflns_number_total             6605
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c9dt04847b2.cif
_cod_data_source_block           t268mcsqma
_cod_depositor_comments
'Adding full bibliography for 7703297--7703299.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7703297
_cell_measurement_2theta_min     2.23
_cell_measurement_2theta_max     49.37
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.77386(2) 0.28500(2) 0.53318(5) 0.04051(15) Uani 1 1 d .
Cl1 Cl 0.70610(14) 0.34371(11) 0.4789(3) 0.0547(9) Uani 1 1 d .
Cl2 Cl 0.86180(13) 0.26079(11) 0.5711(3) 0.0550(8) Uani 1 1 d .
N1 N 0.7721(4) 0.2722(3) 0.6970(9) 0.043(3) Uani 1 1 d .
N2 N 0.7835(3) 0.2986(3) 0.3507(8) 0.036(2) Uani 1 1 d .
C1 C 0.8121(5) 0.2966(4) 0.7991(10) 0.036(3) Uani 1 1 d .
C2 C 0.8025(5) 0.3453(4) 0.8291(10) 0.038(3) Uani 1 1 d .
C3 C 0.8445(5) 0.3677(4) 0.9172(10) 0.042(3) Uani 1 1 d .
H3 H 0.8402 0.4011 0.9385 0.050 Uiso 1 1 calc R
C4 C 0.8902(5) 0.3443(5) 0.9726(10) 0.044(3) Uani 1 1 d .
H4 H 0.9181 0.3613 1.0298 0.053 Uiso 1 1 calc R
C5 C 0.8966(5) 0.2949(5) 0.9457(10) 0.045(3) Uani 1 1 d .
H5 H 0.9286 0.2780 0.9876 0.054 Uiso 1 1 calc R
C6 C 0.8577(5) 0.2698(4) 0.8595(10) 0.040(3) Uani 1 1 d .
C7 C 0.8657(5) 0.2155(5) 0.8353(10) 0.048(3) Uani 1 1 d .
H7 H 0.8405 0.2069 0.7556 0.058 Uiso 1 1 calc R
C8 C 0.9226(5) 0.2029(5) 0.8334(11) 0.064(4) Uani 1 1 d .
H8A H 0.9340 0.2264 0.7818 0.097 Uiso 1 1 calc R
H8B H 0.9233 0.1691 0.8028 0.097 Uiso 1 1 calc R
H8C H 0.9471 0.2050 0.9144 0.097 Uiso 1 1 calc R
C9 C 0.8517(6) 0.1822(5) 0.9296(12) 0.058(4) Uani 1 1 d .
H9A H 0.8756 0.1904 1.0087 0.087 Uiso 1 1 calc R
H9B H 0.8565 0.1472 0.9117 0.087 Uiso 1 1 calc R
H9C H 0.8143 0.1879 0.9281 0.087 Uiso 1 1 calc R
C10 C 0.7512(5) 0.3737(4) 0.7751(11) 0.046(3) Uani 1 1 d .
H10 H 0.7264 0.3518 0.7147 0.055 Uiso 1 1 calc R
C11 C 0.7227(6) 0.3885(5) 0.8653(12) 0.062(4) Uani 1 1 d .
H11A H 0.7167 0.3590 0.9086 0.093 Uiso 1 1 calc R
H11B H 0.6881 0.4038 0.8243 0.093 Uiso 1 1 calc R
H11C H 0.7449 0.4124 0.9217 0.093 Uiso 1 1 calc R
C12 C 0.7605(6) 0.4205(4) 0.7122(11) 0.056(4) Uani 1 1 d .
H12A H 0.7779 0.4456 0.7714 0.084 Uiso 1 1 calc R
H12B H 0.7259 0.4333 0.6625 0.084 Uiso 1 1 calc R
H12C H 0.7837 0.4129 0.6619 0.084 Uiso 1 1 calc R
C13 C 0.7627(5) 0.2617(4) 0.2721(10) 0.039(3) Uani 1 1 d .
C14 C 0.7750(5) 0.2569(4) 0.1628(10) 0.037(3) Uani 1 1 d .
H14 H 0.7612 0.2301 0.1102 0.045 Uiso 1 1 calc R
C15 C 0.8075(4) 0.2919(4) 0.1352(9) 0.043(3) Uani 1 1 d .
H15 H 0.8171 0.2891 0.0632 0.051 Uiso 1 1 calc R
C16 C 0.8266(4) 0.3317(4) 0.2109(10) 0.042(3) Uani 1 1 d .
H16 H 0.8482 0.3566 0.1904 0.050 Uiso 1 1 calc R
C17 C 0.8134(4) 0.3342(4) 0.3169(9) 0.033(3) Uani 1 1 d .
C18 C 0.8315(4) 0.3784(4) 0.3960(9) 0.032(3) Uani 1 1 d .
C19 C 0.7975(5) 0.4190(4) 0.3907(10) 0.034(3) Uani 1 1 d .
C20 C 0.8173(4) 0.4597(3) 0.4640(9) 0.030(3) Uani 1 1 d .
H20 H 0.7942 0.4873 0.4614 0.037 Uiso 1 1 calc R
C21 C 0.8691(5) 0.4616(3) 0.5405(9) 0.035(3) Uani 1 1 d .
C22 C 0.9030(5) 0.4222(4) 0.5392(9) 0.035(3) Uani 1 1 d .
H22 H 0.9392 0.4236 0.5884 0.042 Uiso 1 1 calc R
C23 C 0.8858(4) 0.3800(4) 0.4673(9) 0.035(3) Uani 1 1 d .
C24 C 0.9276(4) 0.3417(4) 0.4636(10) 0.036(3) Uani 1 1 d .
H24 H 0.9083 0.3103 0.4310 0.043 Uiso 1 1 calc R
C25 C 0.9588(5) 0.3582(4) 0.3798(11) 0.053(3) Uani 1 1 d .
H25A H 0.9341 0.3625 0.2995 0.079 Uiso 1 1 calc R
H25B H 0.9858 0.3330 0.3779 0.079 Uiso 1 1 calc R
H25C H 0.9768 0.3898 0.4075 0.079 Uiso 1 1 calc R
C26 C 0.9670(4) 0.3297(4) 0.5871(10) 0.045(3) Uani 1 1 d .
H26A H 0.9895 0.3588 0.6171 0.068 Uiso 1 1 calc R
H26B H 0.9900 0.3017 0.5798 0.068 Uiso 1 1 calc R
H26C H 0.9466 0.3210 0.6426 0.068 Uiso 1 1 calc R
C27 C 0.8881(4) 0.5062(4) 0.6218(9) 0.035(3) Uani 1 1 d .
H27 H 0.8583 0.5311 0.6036 0.042 Uiso 1 1 calc R
C28 C 0.9362(4) 0.5303(3) 0.5993(9) 0.033(3) Uani 1 1 d .
H28A H 0.9671 0.5078 0.6240 0.049 Uiso 1 1 calc R
H28B H 0.9444 0.5612 0.6450 0.049 Uiso 1 1 calc R
H28C H 0.9285 0.5376 0.5142 0.049 Uiso 1 1 calc R
C29 C 0.9001(5) 0.4914(5) 0.7539(10) 0.058(4) Uani 1 1 d .
H29A H 0.9273 0.4651 0.7725 0.088 Uiso 1 1 calc R
H29B H 0.8671 0.4794 0.7688 0.088 Uiso 1 1 calc R
H29C H 0.9136 0.5204 0.8043 0.088 Uiso 1 1 calc R
C30 C 0.7430(5) 0.4214(4) 0.2975(10) 0.042(3) Uani 1 1 d .
H30 H 0.7288 0.3867 0.2853 0.050 Uiso 1 1 calc R
C31 C 0.7014(5) 0.4522(4) 0.3329(12) 0.050(3) Uani 1 1 d .
H31A H 0.7120 0.4873 0.3375 0.075 Uiso 1 1 calc R
H31B H 0.6990 0.4412 0.4108 0.075 Uiso 1 1 calc R
H31C H 0.6664 0.4482 0.2733 0.075 Uiso 1 1 calc R
C32 C 0.7492(5) 0.4389(4) 0.1792(10) 0.045(3) Uani 1 1 d .
H32A H 0.7136 0.4417 0.1209 0.068 Uiso 1 1 calc R
H32B H 0.7709 0.4149 0.1506 0.068 Uiso 1 1 calc R
H32C H 0.7670 0.4713 0.1897 0.068 Uiso 1 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'
W W -0.8490 6.8722 '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
N1 W1 N2 175.1(4) . .
N1 W1 W1 91.4(2) . 7_656
N2 W1 W1 90.5(2) . 7_656
N1 W1 Cl2 93.7(3) . .
N2 W1 Cl2 81.5(2) . .
W1 W1 Cl2 104.20(9) 7_656 .
N1 W1 Cl1 99.1(3) . .
N2 W1 Cl1 85.0(2) . .
W1 W1 Cl1 100.21(9) 7_656 .
Cl2 W1 Cl1 152.09(11) . .
C13 N1 C1 115.4(9) 7_656 .
C13 N1 W1 124.5(7) 7_656 .
C1 N1 W1 120.0(7) . .
C13 N2 C17 117.7(9) . .
C13 N2 W1 113.3(7) . .
C17 N2 W1 128.3(7) . .
C6 C1 C2 123.0(11) . .
C6 C1 N1 118.2(9) . .
C2 C1 N1 118.8(11) . .
C1 C2 C3 115.6(11) . .
C1 C2 C10 124.7(11) . .
C3 C2 C10 119.7(10) . .
C4 C3 C2 123.2(11) . .
C3 C4 C5 119.4(11) . .
C6 C5 C4 121.6(12) . .
C5 C6 C1 117.0(10) . .
C5 C6 C7 119.8(11) . .
C1 C6 C7 123.2(10) . .
C6 C7 C8 113.8(11) . .
C6 C7 C9 110.6(10) . .
C8 C7 C9 108.1(11) . .
C2 C10 C11 113.1(10) . .
C2 C10 C12 112.3(10) . .
C11 C10 C12 107.6(11) . .
N2 C13 N1 117.3(10) . 7_656
N2 C13 C14 122.2(10) . .
N1 C13 C14 120.5(10) 7_656 .
C15 C14 C13 118.0(10) . .
C14 C15 C16 120.8(10) . .
C17 C16 C15 118.5(11) . .
N2 C17 C16 122.5(10) . .
N2 C17 C18 118.8(9) . .
C16 C17 C18 118.7(10) . .
C19 C18 C23 120.8(10) . .
C19 C18 C17 121.0(10) . .
C23 C18 C17 118.0(9) . .
C20 C19 C18 118.2(10) . .
C20 C19 C30 120.7(10) . .
C18 C19 C30 120.7(10) . .
C21 C20 C19 122.8(10) . .
C22 C21 C20 117.9(9) . .
C22 C21 C27 121.4(10) . .
C20 C21 C27 120.7(9) . .
C21 C22 C23 122.2(10) . .
C22 C23 C18 117.9(10) . .
C22 C23 C24 117.5(10) . .
C18 C23 C24 124.4(9) . .
C23 C24 C25 110.2(9) . .
C23 C24 C26 113.8(9) . .
C25 C24 C26 109.6(9) . .
C28 C27 C21 111.5(9) . .
C28 C27 C29 110.7(9) . .
C21 C27 C29 111.1(9) . .
C31 C30 C32 110.7(9) . .
C31 C30 C19 114.6(10) . .
C32 C30 C19 110.3(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N1 1.965(9) .
W1 N2 2.255(9) .
W1 W1 2.2660(11) 7_656
W1 Cl2 2.292(3) .
W1 Cl1 2.314(3) .
N1 C13 1.404(13) 7_656
N1 C1 1.491(14) .
N2 C13 1.356(13) .
N2 C17 1.365(13) .
C1 C6 1.391(15) .
C1 C2 1.401(15) .
C2 C3 1.401(16) .
C2 C10 1.509(16) .
C3 C4 1.336(16) .
C4 C5 1.387(16) .
C5 C6 1.383(15) .
C6 C7 1.516(17) .
C7 C8 1.523(16) .
C7 C9 1.545(17) .
C10 C11 1.510(17) .
C10 C12 1.514(16) .
C13 N1 1.404(13) 7_656
C13 C14 1.414(15) .
C14 C15 1.365(14) .
C15 C16 1.387(15) .
C16 C17 1.383(14) .
C17 C18 1.499(14) .
C18 C19 1.396(14) .
C18 C23 1.415(15) .
C19 C20 1.394(14) .
C19 C30 1.519(15) .
C20 C21 1.386(15) .
C21 C22 1.381(14) .
C21 C27 1.524(13) .
C22 C23 1.409(14) .
C23 C24 1.508(14) .
C24 C25 1.512(15) .
C24 C26 1.546(15) .
C27 C28 1.496(14) .
C27 C29 1.541(15) .
C30 C31 1.512(16) .
C30 C32 1.518(16) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.018 1102 491 ' '
2 0.500 0.500 -0.017 1102 491 ' '
