#------------------------------------------------------------------------------
#$Date: 2021-09-10 02:07:24 +0300 (Fri, 10 Sep 2021) $
#$Revision: 269074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/82/7708266.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_7708266
loop_
_publ_author_name
'Eder, Wolfgang'
'Himmelbauer, Daniel'
'Stöger, Berthold'
'Veiros, Luis F.'
'Pignitter, Marc'
'Kirchner, Karl'
_publ_section_title
;
 Manganese and Iron PCP Pincer Complexes -- The Influence of Sterics on
 Structure and Reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02407H
_journal_year                    2021
_chemical_formula_sum            'C22 H35 Br Fe O2 P2'
_chemical_formula_weight         529.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2190(15)
_cell_length_b                   13.5863(12)
_cell_length_c                   21.3867(19)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.26
_cell_measurement_theta_min      2.17
_cell_volume                     4712.7(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58434
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.602
_diffrn_reflns_theta_min         2.175
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  0.269
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0318
_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/[σ²(Fo²)+(0.0335P)²+1.6157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6117
_reflns_number_total             8605
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02407h2.cif
_cod_data_source_block           4
_cod_database_code               7708266
_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   0.358
_shelx_estimated_absorpt_t_max   0.789
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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_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
Br1 Br 0.54127(2) 0.15459(2) 0.62733(2) 0.01833(5) Uani 1 1 d . . . . .
C1 C 0.37396(10) 0.27082(14) 0.68102(8) 0.0149(3) Uani 1 1 d . . . . .
P1 P 0.51100(3) 0.39010(3) 0.68340(2) 0.01358(9) Uani 1 1 d . . . . .
O1 O 0.56858(8) 0.34879(10) 0.50750(6) 0.0219(3) Uani 1 1 d . . . . .
Fe1 Fe 0.44942(2) 0.30094(2) 0.60737(2) 0.01118(5) Uani 1 1 d . . . . .
C2 C 0.36926(11) 0.33507(14) 0.73265(8) 0.0169(3) Uani 1 1 d . . . . .
O2 O 0.34502(8) 0.46706(10) 0.57938(7) 0.0237(3) Uani 1 1 d . . . . .
P2 P 0.36456(3) 0.19132(3) 0.55935(2) 0.01215(8) Uani 1 1 d . . . . .
C3 C 0.32135(11) 0.31075(16) 0.78501(8) 0.0212(4) Uani 1 1 d . . . . .
H3 H 0.3199 0.3537 0.8201 0.025 Uiso 1 1 calc R U . . .
C4 C 0.27610(11) 0.22425(15) 0.78572(9) 0.0220(4) Uani 1 1 d . . . . .
H4 H 0.2440 0.2077 0.8213 0.026 Uiso 1 1 calc R U . . .
C5 C 0.27778(11) 0.16174(14) 0.73427(9) 0.0191(4) Uani 1 1 d . . . . .
H5 H 0.2458 0.1031 0.7345 0.023 Uiso 1 1 calc R U . . .
C6 C 0.32622(11) 0.18461(13) 0.68219(8) 0.0155(3) Uani 1 1 d . . . . .
C7 C 0.42219(11) 0.42670(14) 0.73099(9) 0.0193(4) Uani 1 1 d . . . . .
H7A H 0.4396 0.4460 0.7736 0.023 Uiso 1 1 calc R U . . .
H7AB H 0.3922 0.4823 0.7115 0.023 Uiso 1 1 calc R U . . .
C8 C 0.32947(12) 0.11700(14) 0.62611(8) 0.0172(3) Uani 1 1 d . . . . .
H8A H 0.2742 0.0891 0.6176 0.021 Uiso 1 1 calc R U . . .
H8AB H 0.3683 0.0621 0.6339 0.021 Uiso 1 1 calc R U . . .
C9 C 0.58079(11) 0.32939(14) 0.74011(8) 0.0182(4) Uani 1 1 d . . . . .
H9 H 0.6265 0.2988 0.7155 0.022 Uiso 1 1 calc R U . . .
C10 C 0.53989(12) 0.24658(15) 0.77799(9) 0.0209(4) Uani 1 1 d . . . . .
H10A H 0.5005 0.2751 0.8077 0.031 Uiso 1 1 calc R U . . .
H10B H 0.5822 0.2099 0.8009 0.031 Uiso 1 1 calc R U . . .
H10C H 0.5108 0.2019 0.7495 0.031 Uiso 1 1 calc R U . . .
C11 C 0.62029(14) 0.40198(16) 0.78588(9) 0.0274(4) Uani 1 1 d . . . . .
H11A H 0.6520 0.4512 0.7625 0.041 Uiso 1 1 calc R U . . .
H11B H 0.6571 0.3663 0.8143 0.041 Uiso 1 1 calc R U . . .
H11C H 0.5771 0.4349 0.8101 0.041 Uiso 1 1 calc R U . . .
C12 C 0.56841(11) 0.50292(13) 0.66189(8) 0.0171(3) Uani 1 1 d . . . . .
H12 H 0.5759 0.5428 0.7008 0.021 Uiso 1 1 calc R U . . .
C13 C 0.52233(12) 0.56657(14) 0.61476(9) 0.0215(4) Uani 1 1 d . . . . .
H13A H 0.5185 0.5316 0.5748 0.032 Uiso 1 1 calc R U . . .
H13B H 0.5521 0.6286 0.6088 0.032 Uiso 1 1 calc R U . . .
H13C H 0.4667 0.5804 0.6304 0.032 Uiso 1 1 calc R U . . .
C14 C 0.65456(12) 0.47774(15) 0.63657(9) 0.0218(4) Uani 1 1 d . . . . .
H14A H 0.6491 0.4408 0.5974 0.033 Uiso 1 1 calc R U . . .
H14B H 0.6842 0.4377 0.6673 0.033 Uiso 1 1 calc R U . . .
H14C H 0.6852 0.5387 0.6288 0.033 Uiso 1 1 calc R U . . .
C15 C 0.40665(11) 0.09782(13) 0.50451(8) 0.0156(3) Uani 1 1 d . . . . .
H15 H 0.4442 0.0556 0.5301 0.019 Uiso 1 1 calc R U . . .
C16 C 0.34058(13) 0.02877(15) 0.47895(10) 0.0272(4) Uani 1 1 d . . . . .
H16A H 0.3066 0.0640 0.4483 0.041 Uiso 1 1 calc R U . . .
H16B H 0.3057 0.0057 0.5134 0.041 Uiso 1 1 calc R U . . .
H16C H 0.3670 -0.0278 0.4587 0.041 Uiso 1 1 calc R U . . .
C17 C 0.45991(12) 0.13936(14) 0.45171(9) 0.0211(4) Uani 1 1 d . . . . .
H17A H 0.4266 0.1834 0.4257 0.032 Uiso 1 1 calc R U . . .
H17B H 0.4810 0.0852 0.4260 0.032 Uiso 1 1 calc R U . . .
H17C H 0.5063 0.1761 0.4696 0.032 Uiso 1 1 calc R U . . .
C18 C 0.26605(11) 0.23178(13) 0.52336(8) 0.0164(3) Uani 1 1 d . . . . .
H18 H 0.2377 0.1707 0.5086 0.020 Uiso 1 1 calc R U . . .
C19 C 0.20762(11) 0.28061(14) 0.57035(9) 0.0192(4) Uani 1 1 d . . . . .
H19A H 0.2335 0.3401 0.5872 0.029 Uiso 1 1 calc R U . . .
H19B H 0.1959 0.2347 0.6045 0.029 Uiso 1 1 calc R U . . .
H19C H 0.1560 0.2983 0.5493 0.029 Uiso 1 1 calc R U . . .
C20 C 0.27890(12) 0.29614(15) 0.46537(9) 0.0217(4) Uani 1 1 d . . . . .
H20A H 0.3112 0.2598 0.4343 0.032 Uiso 1 1 calc R U . . .
H20B H 0.3084 0.3562 0.4772 0.032 Uiso 1 1 calc R U . . .
H20C H 0.2252 0.3136 0.4475 0.032 Uiso 1 1 calc R U . . .
C22 C 0.38615(11) 0.40052(14) 0.59003(8) 0.0166(3) Uani 1 1 d . . . . .
C21 C 0.52178(11) 0.32823(13) 0.54564(8) 0.0159(3) Uani 1 1 d . . . . .
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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
C6 C1 C2 118.21(16) . . ?
C6 C1 Fe1 120.85(13) . . ?
C2 C1 Fe1 120.93(13) . . ?
C7 P1 C12 107.98(9) . . ?
C7 P1 C9 103.73(9) . . ?
C12 P1 C9 102.94(8) . . ?
C7 P1 Fe1 101.40(6) . . ?
C12 P1 Fe1 119.16(6) . . ?
C9 P1 Fe1 120.15(6) . . ?
C22 Fe1 C21 93.89(8) . . ?
C22 Fe1 C1 88.09(8) . . ?
C21 Fe1 C1 176.28(7) . . ?
C22 Fe1 P1 89.84(6) . . ?
C21 Fe1 P1 97.40(6) . . ?
C1 Fe1 P1 79.45(5) . . ?
C22 Fe1 P2 93.22(6) . . ?
C21 Fe1 P2 101.41(6) . . ?
C1 Fe1 P2 81.60(5) . . ?
P1 Fe1 P2 160.69(2) . . ?
C22 Fe1 Br1 177.40(6) . . ?
C21 Fe1 Br1 84.35(6) . . ?
C1 Fe1 Br1 93.77(5) . . ?
P1 Fe1 Br1 92.281(16) . . ?
P2 Fe1 Br1 85.267(16) . . ?
C3 C2 C1 120.63(17) . . ?
C3 C2 C7 121.80(16) . . ?
C1 C2 C7 117.43(15) . . ?
C8 P2 C18 102.60(8) . . ?
C8 P2 C15 103.19(8) . . ?
C18 P2 C15 104.88(8) . . ?
C8 P2 Fe1 101.33(6) . . ?
C18 P2 Fe1 120.95(6) . . ?
C15 P2 Fe1 120.70(6) . . ?
C4 C3 C2 120.13(17) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.94(17) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.38(18) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.62(17) . . ?
C5 C6 C8 121.11(16) . . ?
C1 C6 C8 118.26(15) . . ?
C2 C7 P1 103.64(12) . . ?
C2 C7 H7A 111.0 . . ?
P1 C7 H7A 111.0 . . ?
C2 C7 H7AB 111.0 . . ?
P1 C7 H7AB 111.0 . . ?
H7A C7 H7AB 109.0 . . ?
C6 C8 P2 107.04(12) . . ?
C6 C8 H8A 110.3 . . ?
P2 C8 H8A 110.3 . . ?
C6 C8 H8AB 110.3 . . ?
P2 C8 H8AB 110.3 . . ?
H8A C8 H8AB 108.6 . . ?
C11 C9 C10 108.39(16) . . ?
C11 C9 P1 112.81(13) . . ?
C10 C9 P1 114.03(13) . . ?
C11 C9 H9 107.1 . . ?
C10 C9 H9 107.1 . . ?
P1 C9 H9 107.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 109.83(16) . . ?
C13 C12 P1 112.79(13) . . ?
C14 C12 P1 111.13(13) . . ?
C13 C12 H12 107.6 . . ?
C14 C12 H12 107.6 . . ?
P1 C12 H12 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 111.04(15) . . ?
C16 C15 P2 112.86(13) . . ?
C17 C15 P2 114.90(12) . . ?
C16 C15 H15 105.7 . . ?
C17 C15 H15 105.7 . . ?
P2 C15 H15 105.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C18 C19 111.59(15) . . ?
C20 C18 P2 112.81(12) . . ?
C19 C18 P2 112.86(12) . . ?
C20 C18 H18 106.3 . . ?
C19 C18 H18 106.3 . . ?
P2 C18 H18 106.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C22 Fe1 178.86(17) . . ?
O1 C21 Fe1 177.44(16) . . ?
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
Br1 Fe1 2.5209(3) . ?
C1 C6 1.404(3) . ?
C1 C2 1.410(2) . ?
C1 Fe1 2.0362(17) . ?
P1 C7 1.8325(18) . ?
P1 C12 1.8515(19) . ?
P1 C9 1.8528(18) . ?
P1 Fe1 2.2602(5) . ?
O1 C21 1.149(2) . ?
Fe1 C22 1.7380(19) . ?
Fe1 C21 1.8050(19) . ?
Fe1 P2 2.2731(5) . ?
C2 C3 1.403(3) . ?
C2 C7 1.513(3) . ?
O2 C22 1.146(2) . ?
P2 C8 1.8390(18) . ?
P2 C18 1.8567(18) . ?
P2 C15 1.8588(17) . ?
C3 C4 1.386(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(2) . ?
C5 H5 0.9500 . ?
C6 C8 1.512(2) . ?
C7 H7A 0.9900 . ?
C7 H7AB 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 C11 1.530(3) . ?
C9 C10 1.537(3) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.524(3) . ?
C12 C14 1.537(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.526(3) . ?
C15 C17 1.530(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.532(3) . ?
C18 C19 1.532(2) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
