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_7058656
_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_formula_moiety         'C10 H18 Br2 N4 Ni P2'
_chemical_formula_sum            'C10 H18 Br2 N4 Ni P2'
_chemical_formula_weight         474.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.572(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.0070(14)
_cell_length_b                   8.7064(3)
_cell_length_c                   14.4253(6)
_cell_measurement_reflns_used    27800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     3473.1(3)
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27800
_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         27.513
_diffrn_reflns_theta_min         2.453
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.896
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.525
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+5.7328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3337
_reflns_number_total             3985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03146d1.cif
_cod_data_source_block           me180531Br1_13
_cod_depositor_comments
'Adding full bibliography for 7058649--7058656.cif.'
_cod_database_code               7058656
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.195
_shelx_estimated_absorpt_t_max   0.526
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.349
;
_shelx_res_checksum              1275