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_2020935
_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          '[Mn Br (C19 H35 N P2) (C O)3]'
_chemical_formula_moiety         'C22 H35 Br Mn N O3 P2'
_chemical_formula_sum            'C22 H35 Br Mn N O3 P2'
_chemical_formula_weight         558.30
_chemical_name_systematic
;
{2-[Bis(diisopropylphosphanyl)methyl]-6-methylpyridine-\
\k^2^<i>P</i>,<i>P</i>'}bromidotricarbonylmanganese(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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_cell_formula_units_Z            4
_cell_length_a                   10.6732(5)
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_cell_length_c                   15.1651(7)
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.32
_cell_volume                     2525.9(2)
_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)
;
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_diffrn_measured_fraction_theta_full 1.000
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_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  0.0194
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.873
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.290
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.132
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0327P)^2^+2.4763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                5115
_reflns_number_total             5516
_reflns_threshold_expression     I>2\s(I)
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