#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:15:25 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229817 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/63/7046339.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_7046339
loop_
_publ_author_name
'Hicken, Alexandra'
'White, Andrew J. P.'
'Crimmin, Mark R.'
_publ_section_title
;
 Preparation and characterisation of heterobimetallic copper-tungsten
 hydride complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10595
_journal_page_last               10600
_journal_paper_doi               10.1039/c8dt01569d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H24 Cu F6 N O W, C6 H6'
_chemical_formula_sum            'C30 H30 Cu F6 N O W'
_chemical_formula_weight         781.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.228(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3041(5)
_cell_length_b                   9.7028(5)
_cell_length_c                   13.4827(7)
_cell_measurement_reflns_used    2126
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.5960
_cell_measurement_theta_min      2.6740
_cell_volume                     1450.50(13)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5129
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.604
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.758
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0393
_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)+(0.0235P)²+2.0378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2722
_reflns_number_total             3093
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01569d2.cif
_cod_data_source_block           3-W
_cod_depositor_comments
'Adding full bibliography for 7046336--7046339.cif.'
_cod_original_cell_volume        1450.49(13)
_cod_database_code               7046339
_shelx_shelxl_version_number     2017/1
_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. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
W1 W 0.15984(3) 0.750000 0.49840(2) 0.02784(11) Uani 1 2 d S T P B .
Cu1 Cu 0.04941(8) 0.750000 0.65270(7) 0.0321(2) Uani 1 2 d S T P B .
H1 H 0.110(4) 0.645(5) 0.581(4) 0.034(15) Uiso 1 1 d . . . . .
O1 O -0.1349(5) 0.750000 0.6258(4) 0.0446(15) Uani 1 2 d S T P . .
C1 C -0.1885(7) 0.750000 0.7010(7) 0.037(2) Uani 1 2 d S T P B .
C2 C -0.1455(7) 0.750000 0.8025(6) 0.0340(19) Uani 1 2 d S T P . .
H2A H -0.202686 0.750000 0.845709 0.041 Uiso 1 2 calc R U P B .
C3 C -0.0188(7) 0.750000 0.8495(6) 0.037(2) Uani 1 2 d S T P B .
N3 N 0.0681(5) 0.750000 0.7996(5) 0.0307(15) Uani 1 2 d S T P . .
C4 C -0.3249(8) 0.750000 0.6642(8) 0.050(2) Uani 1 2 d S T P . .
F4A F -0.3879(4) 0.750000 0.7392(4) 0.0690(18) Uani 1 2 d S T P B .
F4B F -0.3626(4) 0.6427(7) 0.6096(5) 0.130(2) Uani 1 1 d . . . . .
C5 C 0.0058(8) 0.750000 0.9639(7) 0.048(2) Uani 1 2 d S T P . .
F5A F -0.0945(5) 0.750000 1.0026(4) 0.082(2) Uani 1 2 d S T P B .
F5B F 0.0679(4) 0.6404(4) 1.0034(3) 0.0651(11) Uani 1 1 d . . . . .
C6 C 0.1933(6) 0.750000 0.8494(6) 0.0251(16) Uani 1 2 d S T P B .
C7 C 0.2538(5) 0.6240(6) 0.8663(4) 0.0297(12) Uani 1 1 d . . . . .
C8 C 0.3771(5) 0.6282(6) 0.9060(4) 0.0313(13) Uani 1 1 d . . . . .
H8A H 0.419580 0.543614 0.919345 0.038 Uiso 1 1 calc R U . . .
C9 C 0.4401(7) 0.750000 0.9267(6) 0.0313(18) Uani 1 2 d S T P . .
C10 C 0.1907(5) 0.4895(6) 0.8398(5) 0.0445(16) Uani 1 1 d . . . . .
H10A H 0.249071 0.413926 0.854595 0.067 Uiso 1 1 calc R U . . .
H10B H 0.154135 0.488648 0.767671 0.067 Uiso 1 1 calc R U . . .
H10C H 0.127744 0.477727 0.879792 0.067 Uiso 1 1 calc R U . . .
C11 C 0.5739(7) 0.750000 0.9732(6) 0.040(2) Uani 1 2 d S T P . .
H11A H 0.584684 0.732017 1.045934 0.060 Uiso 0.5 1 calc R U P A -1
H11B H 0.608596 0.839975 0.962283 0.060 Uiso 0.5 1 calc R U P A -1
H11C H 0.614569 0.678008 0.941388 0.060 Uiso 0.5 1 calc R U P A -1
C21 C -0.0317(5) 0.6782(6) 0.4179(4) 0.0401(15) Uani 1 1 d . . . . .
H21A H -0.087153 0.618164 0.448276 0.048 Uiso 1 1 calc R U . . .
C22 C 0.0567(6) 0.6313(8) 0.3640(5) 0.0536(19) Uani 1 1 d . . . . .
H22A H 0.071088 0.533458 0.346220 0.064 Uiso 1 1 calc R U . B .
C23 C 0.1105(8) 0.750000 0.3299(6) 0.052(3) Uani 1 2 d S T P B .
H23A H 0.168693 0.750001 0.282735 0.063 Uiso 1 2 calc R U P . .
C31 C 0.3309(11) 0.7003(19) 0.6199(7) 0.039(5) Uani 0.5 1 d G U P B -1
H31A H 0.334225 0.638452 0.679662 0.046 Uiso 0.5 1 calc R U P B -1
C32 C 0.3471(16) 0.6592(11) 0.5223(10) 0.045(4) Uani 0.5 1 d G U P B -1
H32A H 0.367995 0.564243 0.502547 0.054 Uiso 0.5 1 calc R U P B -1
C33 C 0.3426(6) 0.7792(14) 0.4614(5) 0.050(5) Uani 0.5 1 d G U P B -1
H33A H 0.360979 0.783259 0.391820 0.060 Uiso 0.5 1 calc R U P B -1
C34 C 0.3236(15) 0.8944(13) 0.5213(10) 0.050(5) Uani 0.5 1 d G U P B -1
H34A H 0.322929 0.993253 0.500098 0.060 Uiso 0.5 1 calc R U P B -1
C35 C 0.3164(10) 0.846(2) 0.6192(7) 0.050(5) Uani 0.5 1 d G U P B -1
H35A H 0.306305 0.903914 0.678205 0.060 Uiso 0.5 1 calc R U P B -1
C41 C 0.4341(10) 0.2962(15) 0.7014(9) 0.062(7) Uani 0.5 1 d G . P C -1
H41A H 0.362156 0.323721 0.656906 0.075 Uiso 0.5 1 calc R U P C -1
C42 C 0.5152(11) 0.3950(11) 0.7481(12) 0.054(6) Uani 0.5 1 d G . P C -1
H42A H 0.498800 0.490054 0.735480 0.065 Uiso 0.5 1 calc R U P C -1
C43 C 0.6205(9) 0.3546(9) 0.8132(9) 0.067(8) Uani 0.5 1 d G . P C -1
H43A H 0.675962 0.422148 0.845068 0.080 Uiso 0.5 1 calc R U P C -1
C44 C 0.6446(10) 0.2155(10) 0.8316(9) 0.070(9) Uani 0.5 1 d G . P C -1
H44A H 0.716483 0.187910 0.876083 0.084 Uiso 0.5 1 calc R U P C -1
C45 C 0.5634(14) 0.1167(9) 0.7849(14) 0.071(7) Uani 0.5 1 d G . P C -1
H45A H 0.579841 0.021575 0.797510 0.086 Uiso 0.5 1 calc R U P C -1
C46 C 0.4582(12) 0.1570(14) 0.7198(11) 0.075(8) Uani 0.5 1 d G . P C -1
H46A H 0.402677 0.089478 0.687922 0.090 Uiso 0.5 1 calc R U P C -1
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
C23 W1 C33 80.3(3) . .
C23 W1 C32 100.8(4) . .
C33 W1 C32 36.84(17) . .
C23 W1 C22 36.8(2) . 4_575
C33 W1 C22 96.4(3) . 4_575
C32 W1 C22 129.4(4) . 4_575
C23 W1 C22 36.8(2) . .
C33 W1 C22 103.9(3) . .
C32 W1 C22 103.8(3) . .
C22 W1 C22 61.0(4) 4_575 .
C23 W1 C34 99.9(4) . .
C33 W1 C34 36.51(19) . .
C32 W1 C34 60.63(12) . .
C22 W1 C34 94.2(4) 4_575 .
C22 W1 C34 133.9(4) . .
C23 W1 C31 136.5(4) . .
C33 W1 C31 60.41(18) . .
C32 W1 C31 36.0(2) . .
C22 W1 C31 153.4(3) 4_575 .
C22 W1 C31 133.1(5) . .
C34 W1 C31 59.61(16) . .
C23 W1 C21 60.0(3) . .
C33 W1 C21 138.5(3) . .
C32 W1 C21 135.2(3) . .
C22 W1 C21 59.6(2) 4_575 .
C22 W1 C21 35.9(2) . .
C34 W1 C21 153.8(3) . .
C31 W1 C21 146.6(4) . .
C23 W1 C21 60.0(3) . 4_575
C33 W1 C21 132.3(3) . 4_575
C32 W1 C21 160.6(4) . 4_575
C22 W1 C21 35.9(2) 4_575 4_575
C22 W1 C21 59.6(2) . 4_575
C34 W1 C21 122.1(3) . 4_575
C31 W1 C21 163.4(4) . 4_575
C21 W1 C21 34.8(3) . 4_575
C23 W1 C35 135.3(4) . .
C33 W1 C35 60.1(2) . .
C32 W1 C35 59.78(12) . .
C22 W1 C35 123.6(5) 4_575 .
C22 W1 C35 162.7(3) . .
C34 W1 C35 35.6(2) . .
C31 W1 C35 35.33(9) . .
C21 W1 C35 161.1(2) . .
C21 W1 C35 135.3(4) 4_575 .
C23 W1 Cu1 138.0(2) . .
C33 W1 Cu1 141.19(18) . .
C32 W1 Cu1 117.7(3) . .
C22 W1 Cu1 112.50(17) 4_575 .
C22 W1 Cu1 112.50(17) . .
C34 W1 Cu1 112.9(3) . .
C31 W1 Cu1 84.3(3) . .
C21 W1 Cu1 80.06(15) . .
C21 W1 Cu1 80.06(15) 4_575 .
C35 W1 Cu1 82.0(2) . .
N3 Cu1 O1 94.9(2) . .
N3 Cu1 W1 146.10(17) . .
O1 Cu1 W1 119.01(17) . .
C1 O1 Cu1 119.0(5) . .
O1 C1 C2 131.7(8) . .
O1 C1 C4 110.4(8) . .
C2 C1 C4 117.9(8) . .
C1 C2 C3 124.7(7) . .
N3 C3 C2 124.0(8) . .
N3 C3 C5 121.5(7) . .
C2 C3 C5 114.6(7) . .
C3 N3 C6 122.3(7) . .
C3 N3 Cu1 125.8(6) . .
C6 N3 Cu1 112.0(5) . .
F4B C4 F4B 106.7(10) . 4_575
F4B C4 F4A 105.2(6) . .
F4B C4 F4A 105.2(6) 4_575 .
F4B C4 C1 112.6(5) . .
F4B C4 C1 112.6(5) 4_575 .
F4A C4 C1 113.9(9) . .
F5B C5 F5B 106.5(8) . 4_575
F5B C5 F5A 105.4(5) . .
F5B C5 F5A 105.4(5) 4_575 .
F5B C5 C3 112.8(5) . .
F5B C5 C3 112.8(5) 4_575 .
F5A C5 C3 113.3(8) . .
C7 C6 C7 122.0(7) . 4_575
C7 C6 N3 118.7(3) . .
C7 C6 N3 118.7(3) 4_575 .
C8 C7 C6 117.3(5) . .
C8 C7 C10 120.7(5) . .
C6 C7 C10 121.9(5) . .
C9 C8 C7 122.7(5) . .
C8 C9 C8 117.8(7) . 4_575
C8 C9 C11 121.1(4) . .
C8 C9 C11 121.1(4) 4_575 .
C21 C21 C22 108.7(4) 4_575 .
C21 C21 W1 72.61(15) 4_575 .
C22 C21 W1 69.6(3) . .
C21 C22 C23 107.1(6) . .
C21 C22 W1 74.5(3) . .
C23 C22 W1 70.2(4) . .
C22 C23 C22 108.4(8) . 4_575
C22 C23 W1 73.0(4) . .
C22 C23 W1 73.0(4) 4_575 .
C35 C31 C32 108.0 . .
C35 C31 W1 73.2(8) . .
C32 C31 W1 69.3(5) . .
C33 C32 C31 108.0 . .
C33 C32 W1 70.8(6) . .
C31 C32 W1 74.7(3) . .
C34 C33 C32 108.0 . .
C34 C33 W1 74.0(8) . .
C32 C33 W1 72.4(8) . .
C33 C34 C35 108.0 . .
C33 C34 W1 69.5(6) . .
C35 C34 W1 74.4(3) . .
C31 C35 C34 108.0 . .
C31 C35 W1 71.5(8) . .
C34 C35 W1 70.1(4) . .
C42 C41 C46 120.0 . .
C41 C42 C43 120.0 . .
C44 C43 C42 120.0 . .
C43 C44 C45 120.0 . .
C44 C45 C46 120.0 . .
C45 C46 C41 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C23 2.231(8) .
W1 C33 2.236(7) .
W1 C32 2.257(18) .
W1 C22 2.269(6) 4_575
W1 C22 2.269(6) .
W1 C34 2.294(19) .
W1 C31 2.328(11) .
W1 C21 2.332(5) .
W1 C21 2.332(5) 4_575
W1 C35 2.350(13) .
W1 Cu1 2.6263(10) .
Cu1 N3 1.951(6) .
Cu1 O1 2.044(5) .
O1 C1 1.279(9) .
C1 C2 1.360(11) .
C1 C4 1.525(12) .
C2 C3 1.449(11) .
C3 N3 1.295(9) .
C3 C5 1.513(12) .
N3 C6 1.443(9) .
C4 F4B 1.298(7) .
C4 F4B 1.298(7) 4_575
C4 F4A 1.345(10) .
C5 F5B 1.328(6) .
C5 F5B 1.328(7) 4_575
C5 F5A 1.337(9) .
C6 C7 1.397(6) .
C6 C7 1.398(6) 4_575
C7 C8 1.392(7) .
C7 C10 1.497(8) .
C8 C9 1.380(7) .
C9 C11 1.520(10) .
C21 C21 1.394(12) 4_575
C21 C22 1.419(8) .
C22 C23 1.421(8) .
C31 C35 1.4200 .
C31 C32 1.4200 .
C32 C33 1.4200 .
C33 C34 1.4200 .
C34 C35 1.4200 .
C41 C42 1.3900 .
C41 C46 1.3900 .
C42 C43 1.3900 .
C43 C44 1.3900 .
C44 C45 1.3900 .
C45 C46 1.3900 .
