#------------------------------------------------------------------------------
#$Date: 2021-04-05 18:10:12 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263807 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/03/7060382.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_7060382
loop_
_publ_author_name
'Mondal, Rajarshi'
'Braun, Jason D.'
'Lozada, Issiah B.'
'Nickel, Rachel'
'van Lierop, Johan'
'Herbert, David E.'
_publ_section_title
;
 Group VIII coordination complexes of bidentate P^N ligands bearing
 π-extended quinoline or phenanthridine N-heterocycles
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4427
_journal_page_last               4436
_journal_paper_doi               10.1039/D1NJ00254F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C52 H40 Br4 Cl4 Fe2 N2 P2'
_chemical_formula_weight         1327.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                107.886(3)
_cell_angle_beta                 110.763(3)
_cell_angle_gamma                97.176(3)
_cell_formula_units_Z            1
_cell_length_a                   10.360(2)
_cell_length_b                   10.778(3)
_cell_length_c                   13.244(3)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.91
_cell_volume                     1269.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation.monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.1439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns.reduction_process narrow--frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.613
_diffrn_reflns_theta_min         2.917
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    4.030
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.0610
_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)+(0.1000P)²+1.1175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4133
_reflns_number_total             7256
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj00254f2.cif
_cod_data_source_block           deh019_raj_sad
_cod_depositor_comments
'Adding full bibliography for 7060382--7060389.cif.'
_cod_database_code               7060382
_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   0.457
_shelx_estimated_absorpt_t_max   0.824
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 1.11753(5) 0.50841(6) 0.93017(4) 0.02210(16) Uani 1 1 d . . . . .
Br2 Br 0.77521(6) 0.71596(6) 0.89652(5) 0.02858(17) Uani 1 1 d . . . . .
Fe1 Fe 0.86653(7) 0.52234(7) 0.86921(6) 0.01466(18) Uani 1 1 d . . . . .
P1 P 0.68568(14) 0.31117(13) 0.74309(11) 0.0159(3) Uani 1 1 d . . . . .
Cl2 Cl 0.7907(2) 0.0915(2) 0.06807(17) 0.0570(5) Uani 1 1 d . . . . .
Cl1 Cl 0.5873(2) 0.2093(2) 0.13903(19) 0.0659(6) Uani 1 1 d . . . . .
N1 N 0.8483(4) 0.5000(4) 0.6915(3) 0.0153(9) Uani 1 1 d . . . . .
C10 C 0.6238(5) 0.3342(5) 0.6054(4) 0.0157(10) Uani 1 1 d . . . . .
C9 C 0.7206(5) 0.4300(5) 0.5953(4) 0.0159(10) Uani 1 1 d . . . . .
C14 C 0.7645(5) 0.1702(5) 0.7198(4) 0.0169(11) Uani 1 1 d . . . . .
C20 C 0.5305(5) 0.2522(5) 0.7654(4) 0.0188(11) Uani 1 1 d . . . . .
C2 C 0.9218(5) 0.6056(5) 0.5781(4) 0.0161(10) Uani 1 1 d . . . . .
C1 C 0.9416(5) 0.5801(5) 0.6807(4) 0.0177(11) Uani 1 1 d . . . . .
H1 H 1.0304 0.6254 0.7466 0.021 Uiso 1 1 calc R U . . .
C11 C 0.4923(6) 0.2663(5) 0.5133(4) 0.0212(12) Uani 1 1 d . . . . .
H11 H 0.4260 0.2039 0.5204 0.025 Uiso 1 1 calc R U . . .
C15 C 0.8399(6) 0.1452(5) 0.8191(5) 0.0240(12) Uani 1 1 d . . . . .
H15 H 0.8450 0.1994 0.8928 0.029 Uiso 1 1 calc R U . . .
C8 C 0.6862(5) 0.4490(5) 0.4889(4) 0.0169(11) Uani 1 1 d . . . . .
C21 C 0.4922(6) 0.3462(6) 0.8395(5) 0.0250(12) Uani 1 1 d . . . . .
H21 H 0.5435 0.4387 0.8729 0.030 Uiso 1 1 calc R U . . .
C6 C 0.7718(6) 0.5703(6) 0.3800(5) 0.0245(12) Uani 1 1 d . . . . .
H6 H 0.6841 0.5288 0.3124 0.029 Uiso 1 1 calc R U . . .
C7 C 0.7902(5) 0.5418(5) 0.4796(4) 0.0176(11) Uani 1 1 d . . . . .
C5 C 0.8788(6) 0.6572(6) 0.3789(5) 0.0271(13) Uani 1 1 d . . . . .
H5 H 0.8640 0.6759 0.3107 0.033 Uiso 1 1 calc R U . . .
C25 C 0.4561(6) 0.1179(6) 0.7176(5) 0.0261(13) Uani 1 1 d . . . . .
H25 H 0.4826 0.0525 0.6675 0.031 Uiso 1 1 calc R U . . .
C3 C 1.0312(6) 0.6941(5) 0.5749(5) 0.0234(12) Uani 1 1 d . . . . .
H3 H 1.1200 0.7362 0.6413 0.028 Uiso 1 1 calc R U . . .
C18 C 0.8311(6) -0.0085(6) 0.6066(5) 0.0299(14) Uani 1 1 d . . . . .
H18 H 0.8299 -0.0604 0.5337 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7605(6) 0.0924(5) 0.6137(4) 0.0217(12) Uani 1 1 d . . . . .
H19 H 0.7092 0.1083 0.5456 0.026 Uiso 1 1 calc R U . . .
C12 C 0.4565(6) 0.2891(6) 0.4098(4) 0.0256(13) Uani 1 1 d . . . . .
H12 H 0.3655 0.2423 0.3470 0.031 Uiso 1 1 calc R U . . .
C4 C 1.0088(6) 0.7189(6) 0.4759(5) 0.0260(13) Uani 1 1 d . . . . .
H4 H 1.0822 0.7784 0.4732 0.031 Uiso 1 1 calc R U . . .
C13 C 0.5504(5) 0.3779(6) 0.3976(4) 0.0212(12) Uani 1 1 d . . . . .
H13 H 0.5238 0.3920 0.3264 0.025 Uiso 1 1 calc R U . . .
C17 C 0.9029(6) -0.0342(6) 0.7040(5) 0.0322(14) Uani 1 1 d . . . . .
H17 H 0.9498 -0.1047 0.6982 0.039 Uiso 1 1 calc R U . . .
C22 C 0.3795(6) 0.3059(7) 0.8652(5) 0.0350(15) Uani 1 1 d . . . . .
H22 H 0.3538 0.3703 0.9167 0.042 Uiso 1 1 calc R U . . .
C16 C 0.9068(7) 0.0425(6) 0.8102(5) 0.0368(15) Uani 1 1 d . . . . .
H16 H 0.9559 0.0243 0.8775 0.044 Uiso 1 1 calc R U . . .
C26 C 0.6479(7) 0.1622(7) 0.0290(5) 0.0398(16) Uani 1 1 d . . . . .
H26A H 0.5688 0.0959 -0.0437 0.048 Uiso 1 1 calc R U . . .
H26B H 0.6781 0.2426 0.0133 0.048 Uiso 1 1 calc R U . . .
C23 C 0.3044(6) 0.1710(8) 0.8153(6) 0.0397(17) Uani 1 1 d . . . . .
H23 H 0.2260 0.1430 0.8318 0.048 Uiso 1 1 calc R U . . .
C24 C 0.3423(6) 0.0791(7) 0.7432(5) 0.0367(15) Uani 1 1 d . . . . .
H24 H 0.2903 -0.0132 0.7097 0.044 Uiso 1 1 calc R U . . .
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'
Fe Fe 0.3463 0.8444 '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'
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
Fe1 Br1 Fe1 93.76(3) . 2_767 ?
N1 Fe1 Br2 94.17(11) . . ?
N1 Fe1 P1 76.27(11) . . ?
Br2 Fe1 P1 114.19(5) . . ?
N1 Fe1 Br1 91.10(11) . . ?
Br2 Fe1 Br1 129.49(4) . . ?
P1 Fe1 Br1 115.85(5) . . ?
N1 Fe1 Br1 167.73(11) . 2_767 ?
Br2 Fe1 Br1 96.78(3) . 2_767 ?
P1 Fe1 Br1 94.12(4) . 2_767 ?
Br1 Fe1 Br1 86.24(3) . 2_767 ?
C14 P1 C20 105.3(2) . . ?
C14 P1 C10 105.1(2) . . ?
C20 P1 C10 108.1(2) . . ?
C14 P1 Fe1 111.48(17) . . ?
C20 P1 Fe1 124.56(18) . . ?
C10 P1 Fe1 100.77(17) . . ?
C1 N1 C9 118.1(4) . . ?
C1 N1 Fe1 119.3(3) . . ?
C9 N1 Fe1 120.1(3) . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 P1 124.8(4) . . ?
C9 C10 P1 115.7(3) . . ?
N1 C9 C8 122.4(5) . . ?
N1 C9 C10 117.6(4) . . ?
C8 C9 C10 120.0(4) . . ?
C19 C14 C15 119.2(5) . . ?
C19 C14 P1 124.6(4) . . ?
C15 C14 P1 116.1(4) . . ?
C25 C20 C21 119.7(5) . . ?
C25 C20 P1 122.7(4) . . ?
C21 C20 P1 117.5(4) . . ?
C3 C2 C7 120.6(4) . . ?
C3 C2 C1 120.6(5) . . ?
C7 C2 C1 118.8(5) . . ?
N1 C1 C2 125.0(4) . . ?
N1 C1 H1 117.5 . . ?
C2 C1 H1 117.5 . . ?
C10 C11 C12 120.2(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C16 C15 C14 120.1(5) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C13 C8 C9 118.2(5) . . ?
C13 C8 C7 123.2(4) . . ?
C9 C8 C7 118.6(4) . . ?
C20 C21 C22 120.2(6) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C5 C6 C7 120.7(5) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C6 C7 C2 117.9(5) . . ?
C6 C7 C8 125.1(5) . . ?
C2 C7 C8 117.0(4) . . ?
C6 C5 C4 121.2(5) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C20 C25 C24 119.5(6) . . ?
C20 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C4 C3 C2 119.6(5) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C17 C18 C19 120.5(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C14 C19 C18 120.0(5) . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C13 C12 C11 120.9(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C3 C4 C5 120.1(5) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C12 C13 C8 121.0(4) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
C18 C17 C16 119.9(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C21 C22 C23 119.6(6) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C15 C16 C17 120.2(5) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
Cl2 C26 Cl1 111.3(3) . . ?
Cl2 C26 H26A 109.4 . . ?
Cl1 C26 H26A 109.4 . . ?
Cl2 C26 H26B 109.4 . . ?
Cl1 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C24 C23 C22 120.2(6) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.9(6) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
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 2.4738(10) . ?
Br1 Fe1 2.7277(10) 2_767 ?
Br2 Fe1 2.3777(10) . ?
Fe1 N1 2.227(4) . ?
Fe1 P1 2.4210(16) . ?
Fe1 Br1 2.7277(10) 2_767 ?
P1 C14 1.808(5) . ?
P1 C20 1.809(5) . ?
P1 C10 1.813(5) . ?
Cl2 C26 1.737(6) . ?
Cl1 C26 1.747(7) . ?
N1 C1 1.290(6) . ?
N1 C9 1.381(6) . ?
C10 C11 1.380(7) . ?
C10 C9 1.418(7) . ?
C9 C8 1.412(6) . ?
C14 C19 1.381(7) . ?
C14 C15 1.398(7) . ?
C20 C25 1.379(7) . ?
C20 C21 1.383(8) . ?
C2 C3 1.408(7) . ?
C2 C7 1.410(7) . ?
C2 C1 1.419(6) . ?
C1 H1 0.9500 . ?
C11 C12 1.395(7) . ?
C11 H11 0.9500 . ?
C15 C16 1.374(8) . ?
C15 H15 0.9500 . ?
C8 C13 1.408(7) . ?
C8 C7 1.441(7) . ?
C21 C22 1.384(8) . ?
C21 H21 0.9500 . ?
C6 C5 1.366(8) . ?
C6 C7 1.399(7) . ?
C6 H6 0.9500 . ?
C5 C4 1.389(8) . ?
C5 H5 0.9500 . ?
C25 C24 1.389(8) . ?
C25 H25 0.9500 . ?
C3 C4 1.364(7) . ?
C3 H3 0.9500 . ?
C18 C17 1.373(8) . ?
C18 C19 1.382(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C12 C13 1.365(8) . ?
C12 H12 0.9500 . ?
C4 H4 0.9500 . ?
C13 H13 0.9500 . ?
C17 C16 1.379(8) . ?
C17 H17 0.9500 . ?
C22 C23 1.385(9) . ?
C22 H22 0.9500 . ?
C16 H16 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C23 C24 1.352(10) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
