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_1557541
_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         'C16 Al F36 O4, C6 I O6 W'
_chemical_formula_sum            'C22 Al F36 I O10 W'
_chemical_formula_weight         1445.95
_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'
_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                90
_cell_angle_beta                 110.764(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4380(6)
_cell_length_b                   28.3511(10)
_cell_length_c                   17.5878(6)
_cell_measurement_reflns_used    9436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.721
_cell_measurement_theta_min      4.458
_cell_volume                     7664.2(5)
_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 0.996
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         1.325
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5572
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.506
_exptl_crystal_description       block
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.15
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_refine_diff_density_min         -2.188
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1273
_refine_ls_number_reflns         15706
_refine_ls_number_restraints     1956
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0598P)^2^+79.7821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13770
_reflns_number_total             15706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06445a2.cif
_cod_data_source_block           p21c_neu_a
_cod_depositor_comments
;

 Adding full bibliography for 1557531--1557542.cif.

2022-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 Al2 F72 I2 O20 W2'
_cod_original_formula_weight         2891.90
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1557541
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              87970