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_2020822
_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 (C O)2]'
_chemical_formula_moiety         'C20 H34 Cl Fe N O2 P2'
_chemical_formula_sum            'C20 H34 Cl Fe N O2 P2'
_chemical_formula_weight         473.72
_chemical_name_systematic
{2,5-Bis[(diisopropylphosphanyl)methyl]pyrrolido-\k^3^<i>P</i>,<i>N</i>,<i>P</i>'}dicarbonylchloridoiron(II)
_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     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.729(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7917(17)
_cell_length_b                   14.6349(18)
_cell_length_c                   11.2225(13)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.29
_cell_volume                     2265.0(5)
_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
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      120.04
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44037
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         2.029
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.475
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0420
_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^)+4.0807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                5123
_reflns_number_total             5626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3121sup1.cif
_cod_data_source_block           III
_cod_database_code               2020822
_shelx_hkl_checksum              4967
_shelx_res_checksum              8523
_cod_database_fobs_code 2020822