Iron pyrrole-based PNP pincer ligand complexes as catalyst precursors
Holland, Amanda M.; Oliver, Allen G.; Iluc, Vlad M.; Acta Crystallographica Section C 73 (2017) 569–574; doi:10.1107/S2053229617009287

data_2020821
_publ_section_title
;
 Iron pyrrole-based PNP pincer ligand complexes as catalyst precursors
;
_journal_coeditor_code           KY3121
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              569
_journal_page_last               574
_journal_paper_doi               10.1107/S2053229617009287
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Fe (C18 H34 N P2) Cl (C5 H5 N)]'
_chemical_formula_moiety         'C23 H39 Cl Fe N2 P2'
_chemical_formula_sum            'C23 H39 Cl Fe N2 P2'
_chemical_formula_weight         496.80
_chemical_name_systematic
{2,5-Bis[(diisopropylphosphanyl)methyl]pyrrolido-\k^3^<i>P</i>,<i>N</i>,<i>P</i>'}chlorido(pyridine-\k<i>N</i>)iron(II)
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.3658(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6074(6)
_cell_length_b                   18.2229(15)
_cell_length_c                   19.1442(16)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.24
_cell_volume                     2651.7(4)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
SAINT (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
olex2.solve (Bourhis <i>et al.</i>, 2015)
;
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44868
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         1.543
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       Block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.597
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.358
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0250P)^2^+1.1820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                5174
_reflns_number_total             5423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3121sup1.cif
_cod_data_source_block           II
_cod_database_code               2020821
_shelx_hkl_checksum              85632
_shelx_res_checksum              27143
_cod_database_fobs_code 2020821