Synthesis and coordination properties of new σ2,λ3-P/N switchable chelators based on [1,2,3]-diazaphosphole
Kozáček, Pavel; Dostál, Libor; Růžička, Aleš; Císařová, Ivana; Černošek, Zdeněk; Erben, Milan; New Journal of Chemistry 43 (2019) 13388–; doi:10.1039/C9NJ03146D

data_7058649
_publ_section_title
;
 Synthesis and coordination properties of new \s2,\l3-P/N switchable
 chelators based on [1,2,3]-diazaphosphole
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13388
_journal_paper_doi               10.1039/C9NJ03146D
_journal_volume                  43
_journal_year                    2019
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C18 H26 N4 O4 P2 Si W'
_chemical_formula_sum            'C18 H26 N4 O4 P2 Si W'
_chemical_formula_weight         636.31
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-05 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.9717(10)
_cell_length_b                   20.3377(9)
_cell_length_c                   21.9312(9)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5286
_cell_measurement_theta_min      2.2464
_cell_volume                     10226.0(8)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service vV6.2.1'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            131565
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.719
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       prism
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.226
_refine_diff_density_max         1.227
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.000215(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         23576
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+11.9338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19672
_reflns_number_total             23576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03146d1.cif
_cod_data_source_block           mo_me160616w1_vinklarek
_cod_depositor_comments
'Adding full bibliography for 7058649--7058656.cif.'
_cod_database_code               7058649
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.232
_shelx_estimated_absorpt_t_max   0.415
_shelx_res_checksum              49408