Crystal structure of NiFe(CO)~5~[tris(pyridylmethyl)azaphosphatrane]: a synthetic mimic of the NiFe hydrogenase active site incorporating a pendant pyridine base
Sutthirat, Natwara; Ziller, Joseph W.; Yang, Jenny Y.; Thammavongsy, Zachary; Acta Crystallographica Section E 75 (2019) 438–442; doi:10.1107/S2056989019003256

data_2242866
_publ_section_title
;
 Crystal structure of NiFe(CO)~5~[tris(pyridylmethyl)azaphosphatrane]: a
 synthetic mimic of the NiFe hydrogenase active site incorporating a
 pendant pyridine base
;
_journal_coeditor_code           SU5488
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              438
_journal_page_last               442
_journal_paper_doi               10.1107/S2056989019003256
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Fe Ni (C24 H30 N7 P) (C O)5]'
_chemical_formula_moiety         'C29 H30 Fe N7 Ni O5 P'
_chemical_formula_sum            'C29 H30 Fe N7 Ni O5 P'
_chemical_formula_weight         702.13
_chemical_name_systematic
Di-\m-carbonyl-tricarbonyl[2,8,9-tris(pyridin-2-ylmethyl)-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane]ironnickel
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 103.1611(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5584(15)
_cell_length_b                   12.9709(17)
_cell_length_c                   20.761(3)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.38
_cell_volume                     3030.8(7)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART 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  0.0264
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34054
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.103
_diffrn_reflns_theta_min         1.809
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+1.4440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                6933
_reflns_number_total             7655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5488sup1.cif
_cod_data_source_block           I
_cod_database_code               2242866
_shelx_estimated_absorpt_t_min   0.675
_shelx_estimated_absorpt_t_max   0.769
_shelx_hkl_checksum              66235
_shelx_res_checksum              39744
_cod_database_fobs_code 2242866