Synthesis and coordination chemistry of the PPN ligand 2-[bis(diisopropylphosphanyl)methyl]-6-methylpyridine
Han, Delong; Andres, Benjamin; Spannenberg, Anke; Beweries, Torsten; Acta Crystallographica Section C 73 (2017) 917–922; doi:10.1107/S205322961701261X

data_2020934
_publ_section_title
;
 Synthesis and coordination chemistry of the PPN ligand
 2-[bis(diisopropylphosphanyl)methyl]-6-methylpyridine
;
_journal_coeditor_code           OV3095
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              917
_journal_page_last               922
_journal_paper_doi               10.1107/S205322961701261X
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Co Cl2 (C19 H35 N P2)]'
_chemical_formula_moiety         'C19 H35 Cl2 Co N P2'
_chemical_formula_sum            'C19 H35 Cl2 Co N P2'
_chemical_formula_weight         469.25
_chemical_name_systematic
{2-[Bis(diisopropylphosphanyl)methyl]-6-methylpyridine-\k^2^<i>P</i>,<i>N</i>}Dichloridocobalt(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                86.8728(10)
_cell_angle_beta                 80.5491(10)
_cell_angle_gamma                75.6607(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2603(2)
_cell_length_b                   10.7220(3)
_cell_length_c                   13.6314(3)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.50
_cell_volume                     1153.68(5)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2015)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.515
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       prism
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.6269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                4435
_reflns_number_total             5055
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ov3095sup1.cif
_cod_data_source_block           3
_cod_database_code               2020934
_shelx_hkl_checksum              47778
_shelx_res_checksum              37472
_cod_database_fobs_code 2020934