Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via the N2S2 Metallo-Ligand Strategy
Yang, X.; Lunsford, A.; Darensbourg, M.Y.; Inorganics 7 (2019) 115–; doi:10.3390/inorganics7090115

data_1556436
_publ_section_title
;
 Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via
 the N2S2 Metallo-Ligand Strategy
;
_journal_name_full               Inorganics
_journal_page_first              115
_journal_paper_doi               10.3390/inorganics7090115
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C14 H18 Cl Ga N2 O5 S2 W'
_chemical_formula_sum            'C14 H18 Cl Ga N2 O5 S2 W'
_chemical_formula_weight         647.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 95.932(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2266(11)
_cell_length_b                   19.245(2)
_cell_length_c                   12.8581(18)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100
_cell_measurement_theta_max      61.28
_cell_measurement_theta_min      4.60
_cell_volume                     2024.8(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Micro-Source CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21370
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        61.262
_diffrn_reflns_theta_max         61.262
_diffrn_reflns_theta_min         4.150
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.370
_exptl_absorpt_correction_T_max  0.1560
_exptl_absorpt_correction_T_min  0.0455
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_description       needle
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0320
_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/[\s^2^(Fo^2^)+(0.0302P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2951
_reflns_number_total             3117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gawco5.cif
_cod_data_source_block           gawco5
_cod_original_cell_volume        2024.8(5)
_cod_database_code               1556436
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.309
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(S2A)
3. Others
 Sof(S2A)=Sof(H14c)=Sof(H14d)=1-FVAR(1)
 Sof(S2)=Sof(H14a)=Sof(H14b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,
 H11b), C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C14(H14c,H14d)
;
_shelx_res_checksum              63407
_shelx_hkl_checksum              4061
_olex2_diffrn_ambient_temperature_device 'Oxford 700'
_olex2_submission_special_instructions 'No special instructions were received'