Completing the triad: synthesis and full characterization of homoleptic and heteroleptic carbonyl and nitrosyl complexes of the group VI metals
Bohnenberger, Jan; Schmitt, Manuel; Feuerstein, Wolfram; Krummenacher, Ivo; Butschke, Burkhard; Czajka, Jakub; Malinowski, Przemysław J.; Breher, Frank; Krossing, Ingo; Chemical Science 11 (2020) 3592–3603; doi:10.1039/C9SC06445A

data_1557539
_publ_section_title
;
 Completing the triad: synthesis and full characterization of homoleptic
 and heteroleptic carbonyl and nitrosyl complexes of the group VI metals
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              3592
_journal_page_last               3603
_journal_paper_doi               10.1039/C9SC06445A
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C24 Al2 F55 O6, C6 I O6 W'
_chemical_formula_sum            'C30 Al2 F55 I O12 W'
_chemical_formula_weight         1962.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2020-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                85.595(2)
_cell_angle_beta                 76.545(3)
_cell_angle_gamma                78.485(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5119(7)
_cell_length_b                   12.5617(8)
_cell_length_c                   21.1226(15)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.437
_cell_measurement_theta_min      4.724
_cell_volume                     2656.7(3)
_computing_cell_refinement       'SAINT V8.38A (1, 2016)'
_computing_data_collection       'APEX2 v2013..6-2'
_computing_data_reduction        'SAINT V8.38A (1, 2016)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  ShelXle-861
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart ApexII Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         0.992
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    3.038
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.013
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         9734
_refine_ls_number_restraints     1431
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+7.1229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7851
_reflns_number_total             9734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06445a2.cif
_cod_data_source_block           p-1_a_CCDC1
_cod_depositor_comments
;Adding full bibliography for 1557531--1557542.cif.

 Adding full bibliography for 1557531--1557542.cif.
;
_cod_database_code               1557539
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              76692