(Et<sub>4</sub>N)[W<sup>III</sup>(DAPBH)(CN)<sub>2</sub>], the first pentagonal-bipyramidal W(III) complex with unquenched orbital angular momentum: a novel Ising-type magnetic building block for single-molecule magnets.
Manakin, Yu V.; Mironov, V. S.; Bazhenova, T. A.; Yakushev, I. A.; Gilmutdinov, I. F.; Simonov, S. V.; Yagubskii, E. B.; Chemical communications (Cambridge, England) 59 (2023) 643–646; doi:10.1039/d2cc05998c

data_7131133
_publ_section_title
;
 (Et<sub>4</sub>N)[W<sup>III</sup>(DAPBH)(CN)<sub>2</sub>], the first
 pentagonal-bipyramidal W(III) complex with unquenched orbital angular
 momentum: a novel Ising-type magnetic building block for single-molecule
 magnets.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              643
_journal_page_last               646
_journal_paper_doi               10.1039/d2cc05998c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C25 H19 N7 O2 W, C8 H20 N'
_chemical_formula_sum            'C33 H39 N8 O2 W'
_chemical_formula_weight         763.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4973(6)
_cell_length_b                   10.7901(3)
_cell_length_c                   13.0307(3)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.23
_cell_measurement_theta_min      2.39
_cell_volume                     3163.18(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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 D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48678
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.656
_diffrn_reflns_theta_min         2.093
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.696
_exptl_absorpt_correction_T_max  0.0739
_exptl_absorpt_correction_T_min  0.0425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 2958 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8125
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0208P)^2^+3.2010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6961
_reflns_number_total             8125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05998c2.cif
_cod_data_source_block           21man2404
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7131131--7131133.cif.
;
_cod_database_code               7131133
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.458
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              67793
_shelx_hkl_checksum              97972