Terminal tungsten pnictide complex formation through pnictaethynolate decarbonylation
Cummins, Christopher; Transue, Wesley J.; Joost, Maximilian; Chem. Commun.  (2017) –; doi:10.1039/C7CC06841G

data_7120662
_publ_section_title
;
 Terminal tungsten pnictide complex formation through pnictaethynolate
 decarbonylation
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06841G
_journal_year                    2017
_chemical_formula_sum            'C64 H106 As Na O12 W'
_chemical_formula_weight         1011.93
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-21 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   57.2329(15)
_cell_length_b                   18.4351(6)
_cell_length_c                   38.9112(11)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      2.20
_cell_volume                     41055(2)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       81
_diffrn_reflns_limit_h_min       -81
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            420443
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_min         2.321
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    2.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             16896
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dimethoxyethane/dioxane/pentane'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.108
_exptl_transmission_factor_max   0.5644
_exptl_transmission_factor_min   0.4477
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
; 
 Flack x determined using 11643 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.0013(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1442
_refine_ls_number_reflns         31327
_refine_ls_number_restraints     4874
_refine_ls_restrained_S_all      1.506
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0178P)^2^+165.1231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                26288
_reflns_number_total             31327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06841g3.cif
_cod_data_source_block           P8_17003
_cod_depositor_comments
;

2023-11-22
Z value fixed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            32
_cod_database_code               7120662
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.599
_shelx_estimated_absorpt_t_max   0.795
_shelx_res_checksum              39619