#------------------------------------------------------------------------------
#$Date: 2023-08-05 01:51:39 +0300 (Sat, 05 Aug 2023) $
#$Revision: 285455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/36/7713659.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_7713659
loop_
_publ_author_name
'Schratzberger, Heiko'
'Liebminger, Lorenzo A.'
'Stöger, Berthold'
'Veiros, Luis F.'
'Kirchner, Karl'
_publ_section_title
;
 Base Metal Complexes featuring a New Pyrazole-Derived PCP-Pincer Ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02111D
_journal_year                    2023
_chemical_formula_sum            'C31 H42 B Cl F4 Fe N2 O2 P2'
_chemical_formula_weight         714.71
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-06-21 deposited with the CCDC.	2023-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.046(3)
_cell_length_b                   20.046(3)
_cell_length_c                   7.9727(17)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.35
_cell_volume                     2774.5(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            49104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.216
_diffrn_reflns_theta_min         2.032
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.246
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0536P)²+0.1094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                4595
_reflns_number_total             5421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02111d3.cif
_cod_data_source_block           Fe2
_cod_original_cell_volume        2774.7(10)
_cod_database_code               7713659
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.985
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.31682(3) 1.0000 0.3333 0.01545(13) Uani 1 2 d S T P . .
Cl1 Cl 0.28820(13) 0.94599(13) 0.6096(4) 0.0271(4) Uani 0.5 1 d . . P . .
P1 P 0.26627(4) 0.87862(4) 0.22552(10) 0.01974(17) Uani 1 1 d . . . . .
F1 F 0.5701(3) 0.9527(3) 0.9659(6) 0.0563(14) Uani 0.5 1 d . . P . .
F2 F 0.6239(3) 1.0751(3) 0.8647(7) 0.0555(14) Uani 0.5 1 d . . P . .
F3 F 0.6498(3) 0.9879(3) 0.7364(7) 0.0466(11) Uani 0.5 1 d . . P . .
F4 F 0.5317(3) 0.9740(3) 0.7195(6) 0.0521(13) Uani 0.5 1 d . . P . .
O1 O 0.1698(2) 1.0000 0.3333 0.0768(19) Uani 1 2 d S T P . .
O2 O 0.2718(5) 0.9313(5) 0.6680(10) 0.054(3) Uani 0.5 1 d . . P . .
N1 N 0.50535(14) 0.96267(13) 0.3572(3) 0.0169(5) Uani 1 1 d . . . . .
C1 C 0.29870(17) 0.82230(17) 0.3491(4) 0.0202(6) Uani 1 1 d . . . . .
C2 C 0.37273(17) 0.85908(16) 0.4212(4) 0.0183(6) Uani 1 1 d . . . . .
C3 C 0.39309(18) 0.82004(17) 0.5379(4) 0.0217(6) Uani 1 1 d . . . . .
H3 H 0.4410 0.8467 0.5951 0.026 Uiso 1 1 calc R U . . .
C4 C 0.3430(2) 0.74185(19) 0.5701(5) 0.0293(7) Uani 1 1 d . . . . .
H4 H 0.3571 0.7150 0.6475 0.035 Uiso 1 1 calc R U . . .
C5 C 0.27246(19) 0.70368(18) 0.4884(4) 0.0289(7) Uani 1 1 d . . . . .
H5 H 0.2395 0.6500 0.5057 0.035 Uiso 1 1 calc R U . . .
C6 C 0.24978(18) 0.74319(17) 0.3818(4) 0.0251(6) Uani 1 1 d . . . . .
H6 H 0.2006 0.7166 0.3299 0.030 Uiso 1 1 calc R U . . .
C7 C 0.42914(16) 0.93926(16) 0.3739(3) 0.0165(5) Uani 1 1 d . . . . .
C8 C 0.41655(19) 1.0000 0.3333 0.0148(7) Uani 1 2 d S T P . .
C9 C 0.54707(18) 0.91962(17) 0.3540(4) 0.0231(6) Uani 1 1 d . . . . .
H9A H 0.5101 0.8643 0.3463 0.035 Uiso 1 1 calc R U . . .
H9B H 0.5775 0.9302 0.4569 0.035 Uiso 1 1 calc R U . . .
H9C H 0.5815 0.9357 0.2565 0.035 Uiso 1 1 calc R U . . .
C10 C 0.29133(18) 0.87014(17) 0.0051(4) 0.0268(7) Uani 1 1 d . . . . .
H10 H 0.2737 0.8995 -0.0662 0.032 Uiso 1 1 calc R U . . .
C11 C 0.37783(19) 0.90545(19) -0.0243(4) 0.0296(7) Uani 1 1 d . . . . .
H11A H 0.3875 0.9031 -0.1440 0.044 Uiso 1 1 calc R U . . .
H11B H 0.3969 0.8766 0.0397 0.044 Uiso 1 1 calc R U . . .
H11C H 0.4046 0.9593 0.0127 0.044 Uiso 1 1 calc R U . . .
C12 C 0.2496(2) 0.7865(2) -0.0589(5) 0.0407(9) Uani 1 1 d . . . . .
H12A H 0.2607 0.7859 -0.1785 0.061 Uiso 1 1 calc R U . . .
H12B H 0.1940 0.7639 -0.0429 0.061 Uiso 1 1 calc R U . . .
H12C H 0.2677 0.7565 0.0038 0.061 Uiso 1 1 calc R U . . .
C13 C 0.15905(18) 0.81785(18) 0.2268(5) 0.0306(7) Uani 1 1 d . . . . .
H13 H 0.1464 0.7647 0.1935 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1240(2) 0.8114(2) 0.3999(5) 0.0395(9) Uani 1 1 d . . . . .
H14A H 0.1282 0.8607 0.4301 0.059 Uiso 1 1 calc R U . . .
H14B H 0.1516 0.7981 0.4827 0.059 Uiso 1 1 calc R U . . .
H14C H 0.0696 0.7711 0.3981 0.059 Uiso 1 1 calc R U . . .
C15 C 0.1234(2) 0.8457(2) 0.0939(6) 0.0436(10) Uani 1 1 d . . . . .
H15A H 0.1415 0.8412 -0.0175 0.065 Uiso 1 1 calc R U . . .
H15B H 0.1389 0.8996 0.1155 0.065 Uiso 1 1 calc R U . . .
H15C H 0.0672 0.8140 0.0987 0.065 Uiso 1 1 calc R U . . .
C16 C 0.2269(3) 1.0000 0.3333 0.0411(14) Uani 1 2 d S T P . .
C17 C 0.2932(4) 0.9608(4) 0.5275(11) 0.0211(13) Uani 0.5 1 d . . P . .
B1 B 0.5961(3) 1.0000 0.8333 0.0291(11) Uani 1 2 d S T P . .
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C17 Fe1 C17 174.6(5) . 5_675 ?
C17 Fe1 C16 87.3(2) . . ?
C17 Fe1 C16 87.3(2) 5_675 . ?
C17 Fe1 C8 92.7(2) . . ?
C17 Fe1 C8 92.7(2) 5_675 . ?
C16 Fe1 C8 180.0 . . ?
C17 Fe1 P1 91.8(2) . 5_675 ?
C17 Fe1 P1 88.7(2) 5_675 5_675 ?
C16 Fe1 P1 95.11(2) . 5_675 ?
C8 Fe1 P1 84.89(2) . 5_675 ?
C17 Fe1 P1 88.7(2) . . ?
C17 Fe1 P1 91.8(2) 5_675 . ?
C16 Fe1 P1 95.11(2) . . ?
C8 Fe1 P1 84.89(2) . . ?
P1 Fe1 P1 169.79(4) 5_675 . ?
C17 Fe1 Cl1 2.0(3) . . ?
C17 Fe1 Cl1 176.5(2) 5_675 . ?
C16 Fe1 Cl1 89.23(5) . . ?
C8 Fe1 Cl1 90.77(5) . . ?
P1 Fe1 Cl1 90.93(5) 5_675 . ?
P1 Fe1 Cl1 89.20(5) . . ?
C17 Fe1 Cl1 176.5(2) . 5_675 ?
C17 Fe1 Cl1 2.0(3) 5_675 5_675 ?
C16 Fe1 Cl1 89.23(5) . 5_675 ?
C8 Fe1 Cl1 90.77(5) . 5_675 ?
P1 Fe1 Cl1 89.21(5) 5_675 5_675 ?
P1 Fe1 Cl1 90.93(5) . 5_675 ?
Cl1 Fe1 Cl1 178.45(11) . 5_675 ?
O2 Cl1 C17 156.3(12) . . ?
O2 Cl1 Fe1 161.2(11) . . ?
C17 Cl1 Fe1 4.9(6) . . ?
C1 P1 C10 104.78(14) . . ?
C1 P1 C13 103.94(15) . . ?
C10 P1 C13 102.77(16) . . ?
C1 P1 Fe1 110.27(10) . . ?
C10 P1 Fe1 117.18(10) . . ?
C13 P1 Fe1 116.47(11) . . ?
B1 F1 F2 58.6(3) . 5_676 ?
B1 F1 F4 57.7(3) . 5_676 ?
F2 F1 F4 96.9(4) 5_676 5_676 ?
B1 F1 F3 56.8(3) . 5_676 ?
F2 F1 F3 97.8(4) 5_676 5_676 ?
F4 F1 F3 87.2(4) 5_676 5_676 ?
B1 F2 F4 64.6(4) . 5_676 ?
B1 F2 F1 58.4(3) . 5_676 ?
F4 F2 F1 107.5(4) 5_676 5_676 ?
B1 F3 F3 56.2(3) . 5_676 ?
B1 F3 F1 51.0(2) . 5_676 ?
F3 F3 F1 90.2(3) 5_676 5_676 ?
F2 F4 B1 57.0(3) 5_676 . ?
F2 F4 F1 99.5(4) 5_676 5_676 ?
B1 F4 F1 51.5(2) . 5_676 ?
Cl1 O2 C17 13.2(7) . . ?
N1 N1 C7 108.28(15) 5_675 . ?
N1 N1 C9 118.83(16) 5_675 . ?
C7 N1 C9 131.9(2) . . ?
C2 C1 C6 118.1(3) . . ?
C2 C1 P1 120.0(2) . . ?
C6 C1 P1 121.8(2) . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 C7 119.9(3) . . ?
C1 C2 C7 119.9(2) . . ?
C4 C3 C2 120.1(3) . . ?
C5 C4 C3 119.6(3) . . ?
C6 C5 C4 120.5(3) . . ?
C5 C6 C1 120.9(3) . . ?
N1 C7 C8 109.7(3) . . ?
N1 C7 C2 121.0(2) . . ?
C8 C7 C2 129.2(3) . . ?
C7 C8 C7 104.0(3) 5_675 . ?
C7 C8 Fe1 127.98(17) 5_675 . ?
C7 C8 Fe1 127.98(17) . . ?
C11 C10 C12 109.0(3) . . ?
C11 C10 P1 113.5(2) . . ?
C12 C10 P1 112.9(2) . . ?
C14 C13 C15 112.2(3) . . ?
C14 C13 P1 113.1(2) . . ?
C15 C13 P1 110.7(2) . . ?
O1 C16 Fe1 180.0 . . ?
Cl1 C17 O2 10.5(5) . . ?
Cl1 C17 Fe1 173.1(9) . . ?
O2 C17 Fe1 176.4(8) . . ?
F1 B1 F1 176.0(7) . 5_676 ?
F1 B1 F2 116.3(4) . . ?
F1 B1 F2 63.0(4) 5_676 . ?
F1 B1 F2 63.0(4) . 5_676 ?
F1 B1 F2 116.3(4) 5_676 5_676 ?
F2 B1 F2 163.2(7) . 5_676 ?
F1 B1 F3 72.2(4) . 5_676 ?
F1 B1 F3 111.3(4) 5_676 5_676 ?
F2 B1 F3 83.1(4) . 5_676 ?
F2 B1 F3 111.3(4) 5_676 5_676 ?
F1 B1 F3 111.3(4) . . ?
F1 B1 F3 72.2(4) 5_676 . ?
F2 B1 F3 111.3(4) . . ?
F2 B1 F3 83.1(3) 5_676 . ?
F3 B1 F3 67.5(5) 5_676 . ?
F1 B1 F4 106.2(4) . . ?
F1 B1 F4 70.8(3) 5_676 . ?
F2 B1 F4 108.5(4) . . ?
F2 B1 F4 58.3(3) 5_676 . ?
F3 B1 F4 167.1(4) 5_676 . ?
F3 B1 F4 102.1(3) . . ?
F1 B1 F4 70.8(3) . 5_676 ?
F1 B1 F4 106.2(4) 5_676 5_676 ?
F2 B1 F4 58.3(3) . 5_676 ?
F2 B1 F4 108.5(4) 5_676 5_676 ?
F3 B1 F4 102.1(3) 5_676 5_676 ?
F3 B1 F4 167.1(4) . 5_676 ?
F4 B1 F4 89.1(5) . 5_676 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C17 1.693(9) . ?
Fe1 C17 1.693(9) 5_675 ?
Fe1 C16 1.803(5) . ?
Fe1 C8 1.999(4) . ?
Fe1 P1 2.2849(8) 5_675 ?
Fe1 P1 2.2849(8) . ?
Fe1 Cl1 2.394(3) . ?
Fe1 Cl1 2.394(3) 5_675 ?
Cl1 O2 0.561(6) . ?
Cl1 C17 0.705(8) . ?
P1 C1 1.844(3) . ?
P1 C10 1.859(3) . ?
P1 C13 1.867(3) . ?
F1 B1 1.339(5) . ?
F1 F2 1.402(7) 5_676 ?
F1 F4 1.616(7) 5_676 ?
F1 F3 1.641(7) 5_676 ?
F2 B1 1.342(5) . ?
F2 F4 1.361(7) 5_676 ?
F2 F1 1.402(7) 5_676 ?
F3 B1 1.441(6) . ?
F3 F3 1.602(11) 5_676 ?
F3 F1 1.641(7) 5_676 ?
F4 F2 1.362(7) 5_676 ?
F4 B1 1.446(6) . ?
F4 F1 1.616(8) 5_676 ?
O1 C16 1.146(7) . ?
O2 C17 1.239(9) . ?
N1 N1 1.351(5) 5_675 ?
N1 C7 1.362(4) . ?
N1 C9 1.472(4) . ?
C1 C2 1.408(4) . ?
C1 C6 1.411(4) . ?
C2 C3 1.401(4) . ?
C2 C7 1.479(4) . ?
C3 C4 1.399(4) . ?
C4 C5 1.388(5) . ?
C5 C6 1.384(5) . ?
C7 C8 1.399(4) . ?
C8 C7 1.399(4) 5_675 ?
C10 C11 1.528(4) . ?
C10 C12 1.539(4) . ?
C13 C14 1.525(6) . ?
C13 C15 1.530(5) . ?
B1 F1 1.339(5) 5_676 ?
B1 F2 1.342(5) 5_676 ?
B1 F3 1.441(6) 5_676 ?
B1 F4 1.446(6) 5_676 ?
