#------------------------------------------------------------------------------
#$Date: 2017-07-28 04:20:48 +0200 (Fri 28 de Jul de 2017) $
#$Revision: 199378 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/38/7043848.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_7043848
loop_
_publ_author_name
'Sengupta, Arunava'
'Rajput, Amit'
'Barman, Suman K.'
'Mukherjee, Rabi'
_publ_section_title
;
 Low-spin [MII(L)2] and [MIII(L)2]+ (M = Fe and Co) complexes of
 tridentate azo-containing pyridine/pyrazine amide ligands: structures,
 properties and redox potential correlations
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01577A
_journal_year                    2017
_chemical_formula_moiety         'C36 H26 Fe N8 O2, 0.5(B2 F8)'
_chemical_formula_sum            'C36 H26 B F4 Fe N8 O2'
_chemical_formula_weight         745.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.05.22 svn.r3414 for OlexSys, GUI svn.r5347)
;
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.882(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.714(2)
_cell_length_b                   24.385(2)
_cell_length_c                   11.8024(13)
_cell_measurement_reflns_used    2235
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.54
_cell_volume                     3809.9(7)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19603
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0678 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.2956.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0927
_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)+(0.1660P)²+11.6420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2235
_reflns_number_total             3443
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01577a2.cif
_cod_data_source_block           19juna_a_complex5
_cod_original_cell_volume        3810.0(8)
_cod_database_code               7043848
_shelx_shelxl_version_number     2016/6
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 N3, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed U11: F3(0.119231) F2(0.198794) F1(0.175955) B1(0.071281)
 Fixed U12: F3(0) F2(0) F1(-0.053432) B1(0)
 Fixed U13: F3(0.020081) F2(0.025178) F1(-0.012493) B1(0.016908)
 Fixed U22: F3(0.07111) F2(0.20152) F1(0.2582) B1(0.05399)
 Fixed U23: F3(0) F2(0) F1(0.01114) B1(0)
 Fixed U33: F3(0.28027) F2(0.19412) F1(0.19935) B1(0.14842)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C14(H14), C15(H15), C8(H8), C16(H16), C9(H9), C11(H11), C10(H10),
 C17(H17), C2(H2), C18(H18), C4(H4), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.500000 0.72986(4) 0.500000 0.0251(4) Uani 1 2 d S T P
N2 N 0.4493(4) 0.72838(19) 0.3219(4) 0.0336(12) Uani 1 1 d . . .
N1 N 0.4030(3) 0.66895(18) 0.4692(4) 0.0311(11) Uani 1 1 d . . .
N4 N 0.5983(4) 0.7868(2) 0.5109(6) 0.0444(13) Uani 1 1 d . U .
C7 C 0.4526(4) 0.7718(2) 0.2513(5) 0.0306(13) Uani 1 1 d . . .
C12 C 0.5197(4) 0.8157(3) 0.3135(6) 0.0390(14) Uani 1 1 d . U .
N3 N 0.5954(4) 0.8196(3) 0.4362(5) 0.0565(16) Uani 1 1 d . U .
C13 C 0.6925(5) 0.8017(3) 0.6366(6) 0.0418(15) Uani 1 1 d . U .
C1 C 0.3772(5) 0.6443(2) 0.5519(7) 0.0423(16) Uani 1 1 d . . .
H1 H 0.401295 0.657543 0.633738 0.051 Uiso 1 1 calc R . .
C14 C 0.7625(4) 0.7615(3) 0.6884(5) 0.0353(15) Uani 1 1 d . . .
H14 H 0.755569 0.728445 0.645974 0.042 Uiso 1 1 calc R . .
O1 O 0.3801(5) 0.6650(2) 0.1593(4) 0.084(2) Uani 1 1 d . . .
C5 C 0.3710(5) 0.6477(3) 0.3531(6) 0.0404(16) Uani 1 1 d . . .
C15 C 0.8434(4) 0.7696(3) 0.8028(5) 0.0368(15) Uani 1 1 d . . .
H15 H 0.891570 0.742243 0.839121 0.044 Uiso 1 1 calc R . .
C8 C 0.3915(5) 0.7783(3) 0.1228(6) 0.0383(15) Uani 1 1 d . . .
H8 H 0.348814 0.749996 0.077271 0.046 Uiso 1 1 calc R . .
C16 C 0.8519(5) 0.8199(3) 0.8641(6) 0.053(2) Uani 1 1 d . . .
H16 H 0.905854 0.826199 0.942277 0.064 Uiso 1 1 calc R . .
C9 C 0.3937(5) 0.8264(3) 0.0625(6) 0.0483(18) Uani 1 1 d . . .
H9 H 0.350397 0.830315 -0.022622 0.058 Uiso 1 1 calc R . .
C11 C 0.5219(5) 0.8636(3) 0.2477(7) 0.0505(18) Uani 1 1 d . . .
H11 H 0.567232 0.891569 0.289201 0.061 Uiso 1 1 calc R . .
C6 C 0.3993(5) 0.6802(3) 0.2645(6) 0.0485(18) Uani 1 1 d . . .
C10 C 0.4579(6) 0.8687(3) 0.1241(7) 0.0536(19) Uani 1 1 d . . .
H10 H 0.457433 0.900764 0.081049 0.064 Uiso 1 1 calc R . .
C17 C 0.7800(6) 0.8601(3) 0.8081(9) 0.062(2) Uani 1 1 d . . .
H17 H 0.785344 0.893510 0.848611 0.074 Uiso 1 1 calc R . .
C2 C 0.3123(5) 0.5974(3) 0.5141(9) 0.059(2) Uani 1 1 d . . .
H2 H 0.292084 0.580446 0.569936 0.071 Uiso 1 1 calc R . .
C18 C 0.7009(6) 0.8508(3) 0.6931(7) 0.0513(18) Uani 1 1 d . . .
H18 H 0.653243 0.878049 0.654086 0.062 Uiso 1 1 calc R . .
C4 C 0.3117(6) 0.6024(3) 0.3122(7) 0.059(2) Uani 1 1 d . . .
H4 H 0.292952 0.588338 0.231808 0.071 Uiso 1 1 calc R . .
F3 F 0.7046(9) 1.000000 0.6191(13) 0.157 Uani 1 2 d S T P
C3 C 0.2806(5) 0.5781(3) 0.3945(9) 0.063(2) Uani 1 1 d . . .
H3 H 0.237330 0.548110 0.368172 0.075 Uiso 1 1 calc R . .
F2 F 0.5995(12) 1.000000 0.3937(14) 0.198 Uani 1 2 d S T P
F1 F 0.5505(6) 0.9526(4) 0.5169(10) 0.211 Uani 1 1 d . . .
B1 B 0.6013(15) 1.000000 0.513(2) 0.091 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'
F F 0.0171 0.0103 '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'
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'
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
N2 Fe1 N2 177.8(3) 2_656 .
N2 Fe1 N1 83.1(2) . .
N2 Fe1 N1 83.1(2) 2_656 2_656
N2 Fe1 N1 95.3(2) 2_656 .
N2 Fe1 N1 95.3(2) . 2_656
N2 Fe1 N4 91.0(2) 2_656 .
N2 Fe1 N4 91.0(2) . 2_656
N2 Fe1 N4 90.5(2) . .
N2 Fe1 N4 90.5(2) 2_656 2_656
N1 Fe1 N1 82.8(3) 2_656 .
N4 Fe1 N1 93.8(2) 2_656 .
N4 Fe1 N1 172.4(2) . .
N4 Fe1 N1 172.4(2) 2_656 2_656
N4 Fe1 N1 93.8(2) . 2_656
N4 Fe1 N4 90.3(3) . 2_656
C7 N2 Fe1 124.1(4) . .
C7 N2 C6 120.7(5) . .
C6 N2 Fe1 115.0(4) . .
C1 N1 Fe1 128.0(4) . .
C1 N1 C5 119.1(5) . .
C5 N1 Fe1 112.3(4) . .
N3 N4 Fe1 130.2(5) . .
N3 N4 C13 106.2(6) . .
C13 N4 Fe1 123.1(4) . .
N2 C7 C12 118.1(5) . .
N2 C7 C8 125.2(5) . .
C8 C7 C12 116.6(5) . .
N3 C12 C7 130.4(6) . .
N3 C12 C11 108.4(6) . .
C11 C12 C7 121.1(6) . .
N4 N3 C12 118.9(7) . .
C14 C13 N4 116.2(6) . .
C18 C13 N4 121.7(6) . .
C18 C13 C14 122.0(6) . .
N1 C1 H1 120.1 . .
N1 C1 C2 119.8(7) . .
C2 C1 H1 120.1 . .
C13 C14 H14 120.0 . .
C13 C14 C15 120.1(6) . .
C15 C14 H14 120.0 . .
N1 C5 C6 115.2(5) . .
N1 C5 C4 124.1(7) . .
C4 C5 C6 120.6(6) . .
C14 C15 H15 120.7 . .
C14 C15 C16 118.6(6) . .
C16 C15 H15 120.7 . .
C7 C8 H8 119.7 . .
C9 C8 C7 120.6(6) . .
C9 C8 H8 119.7 . .
C15 C16 H16 120.1 . .
C17 C16 C15 119.8(6) . .
C17 C16 H16 120.1 . .
C8 C9 H9 118.9 . .
C10 C9 C8 122.1(6) . .
C10 C9 H9 118.9 . .
C12 C11 H11 120.1 . .
C10 C11 C12 119.8(7) . .
C10 C11 H11 120.1 . .
N2 C6 C5 110.6(5) . .
O1 C6 N2 126.5(7) . .
O1 C6 C5 122.8(6) . .
C9 C10 H10 120.2 . .
C11 C10 C9 119.7(7) . .
C11 C10 H10 120.2 . .
C16 C17 H17 120.0 . .
C18 C17 C16 119.9(7) . .
C18 C17 H17 120.0 . .
C1 C2 H2 120.7 . .
C3 C2 C1 118.6(7) . .
C3 C2 H2 120.7 . .
C13 C18 C17 119.6(6) . .
C13 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
C5 C4 H4 121.3 . .
C5 C4 C3 117.3(7) . .
C3 C4 H4 121.3 . .
C2 C3 C4 121.0(7) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
F1 F1 B1 121.7(8) 2_656 .
F2 B1 F3 114.2(15) . .
F1 B1 F3 109.9(11) . .
F1 B1 F3 109.9(11) 6_575 .
F1 B1 F2 105.0(12) 6_575 .
F1 B1 F2 105.0(12) . .
F1 B1 F1 112.9(15) . 6_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.899(5) 2_656
Fe1 N2 1.899(5) .
Fe1 N1 1.980(5) .
Fe1 N1 1.980(5) 2_656
Fe1 N4 1.968(6) .
Fe1 N4 1.968(6) 2_656
N2 C7 1.362(7) .
N2 C6 1.395(8) .
N1 C1 1.334(8) .
N1 C5 1.344(7) .
N4 N3 1.178(8) .
N4 C13 1.568(8) .
C7 C12 1.423(9) .
C7 C8 1.394(8) .
C12 N3 1.393(8) .
C12 C11 1.411(9) .
C13 C14 1.359(9) .
C13 C18 1.349(10) .
C1 H1 0.9300 .
C1 C2 1.431(9) .
C14 H14 0.9300 .
C14 C15 1.370(8) .
O1 C6 1.205(8) .
C5 C6 1.507(10) .
C5 C4 1.360(9) .
C15 H15 0.9300 .
C15 C16 1.403(9) .
C8 H8 0.9300 .
C8 C9 1.380(9) .
C16 H16 0.9300 .
C16 C17 1.381(11) .
C9 H9 0.9300 .
C9 C10 1.373(10) .
C11 H11 0.9300 .
C11 C10 1.354(10) .
C10 H10 0.9300 .
C17 H17 0.9300 .
C17 C18 1.367(10) .
C2 H2 0.9300 .
C2 C3 1.362(11) .
C18 H18 0.9300 .
C4 H4 0.9300 .
C4 C3 1.375(11) .
F3 B1 1.49(2) .
C3 H3 0.9300 .
F2 B1 1.40(2) .
F1 F1 1.360(16) 2_656
F1 B1 1.388(12) .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 -0.552 0.000 -0.987 471.6 149.0
2 -0.954 0.500 -0.214 471.6 149.0
