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#$Date: 2025-08-21 15:03:24 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301848 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/89/7028907.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7028907
loop_
_publ_author_name
'Orthaber, Andreas'
'Karnahl, Michael'
'Tschierlei, Stefanie'
'Streich, Daniel'
'Stein, Matthias'
'Ott, Sascha'
_publ_section_title
;
 Coordination and conformational isomers in mononuclear iron complexes
 with pertinence to the [FeFe] hydrogenase active site.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4537
_journal_page_last               4549
_journal_paper_doi               10.1039/c3dt53268b
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C30 H32 N2 P2'
_chemical_formula_sum            'C30 H32 N2 P2'
_chemical_formula_weight         482.52
_space_group_IT_number           32
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2ab'
_symmetry_space_group_name_H-M   'P b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3653(2)
_cell_length_b                   26.2717(7)
_cell_length_c                   5.22710(10)
_cell_measurement_reflns_used    6851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.31
_cell_volume                     1286.09(5)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, )'
_computing_data_collection       'APEX2  (Bruker AXS, 1)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, )'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart ApexII'
_diffrn_measurement_method       'ω -scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6851
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.8943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(9)
_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     154
_refine_ls_number_reflns         2584
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0501P)²+0.0764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                2423
_reflns_number_total             2584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53268b.txt
_cod_data_source_block           Ligand_2b
_cod_database_code               7028907
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
P1 P 0.85406(4) 0.942089(13) 0.47104(9) 0.03219(12) Uani 1 1 d .
N1 N 0.84946(12) 1.04830(5) 0.4092(3) 0.0340(4) Uani 1 1 d .
C5 C 0.8180(2) 0.74129(7) 0.4491(6) 0.0613(5) Uani 1 1 d .
H5 H 0.8363 0.7065 0.4867 0.074 Uiso 1 1 calc R
C4 C 0.8835(2) 0.76400(7) 0.2466(5) 0.0612(6) Uani 1 1 d .
H4 H 0.9486 0.7452 0.1441 0.073 Uiso 1 1 calc R
C3 C 0.8554(2) 0.81457(7) 0.1896(5) 0.0518(5) Uani 1 1 d .
H3 H 0.8996 0.8298 0.0449 0.062 Uiso 1 1 calc R
C2 C 0.76397(18) 0.84335(6) 0.3399(4) 0.0422(4) Uani 1 1 d .
C1 C 0.73749(17) 0.89867(6) 0.2841(4) 0.0433(4) Uani 1 1 d .
H1B H 0.6365 0.9067 0.3226 0.052 Uiso 1 1 calc R
H1A H 0.7532 0.9049 0.0995 0.052 Uiso 1 1 calc R
C8 C 0.80204(18) 1.00113(6) 0.2948(4) 0.0364(4) Uani 1 1 d .
H8A H 0.8411 0.9991 0.1191 0.044 Uiso 1 1 calc R
H8B H 0.6967 1.0020 0.2807 0.044 Uiso 1 1 calc R
C9 C 1.02470(15) 0.92765(6) 0.3018(3) 0.0351(3) Uani 1 1 d .
H9B H 1.0393 0.8903 0.3027 0.042 Uiso 1 1 calc R
H9A H 1.0152 0.9384 0.1211 0.042 Uiso 1 1 calc R
C7 C 0.6985(2) 0.81968(7) 0.5448(4) 0.0547(5) Uani 1 1 d .
H7 H 0.6344 0.8384 0.6497 0.066 Uiso 1 1 calc R
C10 C 0.77517(15) 1.07078(6) 0.6068(4) 0.0304(3) Uani 1 1 d .
C11 C 0.82087(16) 1.11628(6) 0.7213(3) 0.0356(4) Uani 1 1 d .
H11 H 0.9070 1.1318 0.6651 0.043 Uiso 1 1 calc R
C12 C 0.74233(17) 1.13902(6) 0.9152(4) 0.0407(4) Uani 1 1 d .
H12 H 0.7759 1.1697 0.9908 0.049 Uiso 1 1 calc R
C13 C 0.61674(17) 1.11781(6) 0.9994(4) 0.0454(4) Uani 1 1 d .
H13 H 0.5619 1.1340 1.1289 0.054 Uiso 1 1 calc R
C14 C 0.57201(17) 1.07273(6) 0.8923(4) 0.0451(5) Uani 1 1 d .
H14 H 0.4860 1.0576 0.9512 0.054 Uiso 1 1 calc R
C15 C 0.64882(15) 1.04906(6) 0.7020(4) 0.0377(4) Uani 1 1 d .
H15 H 0.6160 1.0176 0.6341 0.045 Uiso 1 1 calc R
C6 C 0.7254(3) 0.76874(8) 0.5990(5) 0.0641(6) Uani 1 1 d .
H6 H 0.6796 0.7529 0.7402 0.077 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 P1 C9 97.43(8) . .
C1 P1 C8 95.58(8) . .
C9 P1 C8 99.11(8) . .
C10 N1 C8 121.47(13) . .
C10 N1 C9 120.91(13) . 2_775
C8 N1 C9 117.58(14) . 2_775
C4 C5 C6 119.88(19) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C5 C4 C3 120.1(2) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C2 C3 C4 121.2(2) . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
C7 C2 C3 117.89(18) . .
C7 C2 C1 120.81(18) . .
C3 C2 C1 121.31(18) . .
C2 C1 P1 113.27(11) . .
C2 C1 H1B 108.9 . .
P1 C1 H1B 108.9 . .
C2 C1 H1A 108.9 . .
P1 C1 H1A 108.9 . .
H1B C1 H1A 107.7 . .
N1 C8 P1 115.31(12) . .
N1 C8 H8A 108.4 . .
P1 C8 H8A 108.4 . .
N1 C8 H8B 108.4 . .
P1 C8 H8B 108.4 . .
H8A C8 H8B 107.5 . .
N1 C9 P1 115.09(11) 2_775 .
N1 C9 H9B 108.5 2_775 .
P1 C9 H9B 108.5 . .
N1 C9 H9A 108.5 2_775 .
P1 C9 H9A 108.5 . .
H9B C9 H9A 107.5 . .
C2 C7 C6 120.7(2) . .
C2 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
N1 C10 C11 122.04(14) . .
N1 C10 C15 121.10(15) . .
C11 C10 C15 116.86(16) . .
C12 C11 C10 121.10(15) . .
C12 C11 H11 119.5 . .
C10 C11 H11 119.5 . .
C13 C12 C11 120.88(16) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C12 C13 C14 118.67(17) . .
C12 C13 H13 120.7 . .
C14 C13 H13 120.7 . .
C13 C14 C15 121.61(16) . .
C13 C14 H14 119.2 . .
C15 C14 H14 119.2 . .
C14 C15 C10 120.84(16) . .
C14 C15 H15 119.6 . .
C10 C15 H15 119.6 . .
C5 C6 C7 120.2(2) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C1 1.8567(17) .
P1 C9 1.8655(16) .
P1 C8 1.8686(16) .
N1 C10 1.378(2) .
N1 C8 1.446(2) .
N1 C9 1.4502(19) 2_775
C5 C4 1.362(3) .
C5 C6 1.373(3) .
C5 H5 0.9500 .
C4 C3 1.387(3) .
C4 H4 0.9500 .
C3 C2 1.386(3) .
C3 H3 0.9500 .
C2 C7 1.382(3) .
C2 C1 1.503(2) .
C1 H1B 0.9900 .
C1 H1A 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 N1 1.4502(19) 2_775
C9 H9B 0.9900 .
C9 H9A 0.9900 .
C7 C6 1.391(3) .
C7 H7 0.9500 .
C10 C11 1.404(2) .
C10 C15 1.405(2) .
C11 C12 1.388(2) .
C11 H11 0.9500 .
C12 C13 1.374(2) .
C12 H12 0.9500 .
C13 C14 1.375(3) .
C13 H13 0.9500 .
C14 C15 1.376(3) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C6 H6 0.9500 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 15889301
