Preparation and characterisation of heterobimetallic copper-tungsten hydride complexes.
Hicken, Alexandra; White, Andrew J. P.; Crimmin, Mark R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10595–10600; doi:10.1039/c8dt01569d

data_7046336
_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         'C33 H35 Cu F6 N2 W'
_chemical_formula_sum            'C33 H35 Cu F6 N2 W'
_chemical_formula_weight         821.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.5350(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.6872(2)
_cell_length_b                   21.27381(17)
_cell_length_c                   15.15393(18)
_cell_measurement_reflns_used    11392
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.6910
_cell_measurement_theta_min      3.7250
_cell_volume                     6245.41(12)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20248
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.908
_diffrn_reflns_theta_min         3.744
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.082
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.298
_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            'Dark red'
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.675
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.000131(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         12120
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.2658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10152
_reflns_number_total             12120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01569d2.cif
_cod_data_source_block           1-W
_cod_depositor_comments
'Adding full bibliography for 7046336--7046339.cif.'
_cod_original_cell_volume        6245.42(12)
_cod_database_code               7046336
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              28742