#------------------------------------------------------------------------------
#$Date: 2021-11-06 19:53:18 +0100 (Sat 06 de Nov de 2021) $
#$Revision: 270380 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/91/7129108.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_7129108
loop_
_publ_author_name
'Taylor, Lauren L. K.'
'Vitorica-Yrezabal, Iñigo J'
'Borilović, Ivana'
'Tuna, Floriana'
'Riddell, Imogen A.'
_publ_section_title
;
 Self-assembly of a trigonal bipyramidal architecture with stabilisation
 of iron in three spin states.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11252
_journal_page_last               11255
_journal_paper_doi               10.1039/d1cc04413c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C20.63 H19.53 Br0.05 N3.95 O1.91'
_chemical_formula_sum            'C20.62 H19.53 Br0.05 N3.96 O1.9'
_chemical_formula_weight         356.88
_chemical_name_systematic        AIR3
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                75.420(14)
_cell_angle_beta                 86.542(13)
_cell_angle_gamma                79.753(14)
_cell_formula_units_Z            2
_cell_length_a                   8.3959(14)
_cell_length_b                   10.4913(17)
_cell_length_c                   10.5635(18)
_cell_measurement_reflns_used    1526
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      26.7950
_cell_measurement_theta_min      3.1320
_cell_volume                     886.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  90.00   1.00    7.50    --   20.02  77.00  30.00  101
  2  ω    -10.00  90.00   1.00    7.50    --   20.02  77.00 150.00  100
  3  ω    -10.00  90.00   1.00    7.50    --   20.02  77.00 -90.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0053209000
_diffrn_orient_matrix_UB_12      0.0668469000
_diffrn_orient_matrix_UB_13      -0.0005011000
_diffrn_orient_matrix_UB_21      -0.0854914000
_diffrn_orient_matrix_UB_22      0.0148828000
_diffrn_orient_matrix_UB_23      0.0059034000
_diffrn_orient_matrix_UB_31      0.0059320000
_diffrn_orient_matrix_UB_32      -0.0182390000
_diffrn_orient_matrix_UB_33      0.0691367000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4679
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_preparation       'In chloroform'
_exptl_crystal_recrystallization_method 'Slow evaporation of cloroform'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3224
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0797
_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)+(0.1060P)²+0.2780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2028
_reflns_number_total             3224
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc04413c2.cif
_cod_data_source_block           air3
_cod_depositor_comments
'Adding full bibliography for 7129106--7129112.cif.'
_cod_original_formula_sum        'C20.62 H19.53 Br0.05 N3.96 O1.90'
_cod_database_code               7129108
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C19 H14 N4 O'
_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_max   0.963
_shelx_estimated_absorpt_t_min   0.963
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Br0 \\sim C008: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Others
 Sof(Br0)=1-FVAR(1)
 Sof(O001)=Sof(O002)=Sof(C008)=Sof(C00K)=Sof(H00K)=Sof(C00N)=Sof(H00N)=
 Sof(C00E)=Sof(N003)=Sof(C007)=Sof(H007)=Sof(C00I)=Sof(H00I)=Sof(C00L)=
 Sof(H00A)=Sof(H00B)=Sof(H00D)=Sof(C00P)=Sof(H00E)=Sof(H00F)=Sof(H00L)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C00I(H00I)
4.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00N(H00N), C007(H007), C00C(H00C), C00G(H00G), C00H(H00H),
 C00J(H00J), C00M(H00M), C00O(H00O), C00Q(H00Q)
4.c Fitted hexagon refined as free rotating group:
 C008(C00K,C00N,C00E,N003,C007)
4.d Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00D), C00P(H00E,H00F,H00L), C00R(H00P,H00R,H00S)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.664
_oxdiff_exptl_absorpt_empirical_full_min 0.736
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
O001 O -0.3759(3) 0.6072(2) 0.1397(2) 0.0396(7) Uani 0.9532(18) 1 d . . P A 1
O002 O -0.1836(3) 0.4190(2) 0.1275(3) 0.0427(7) Uani 0.9532(18) 1 d . . P A 1
N004 N 0.6747(3) 0.8134(3) 0.6524(3) 0.0377(7) Uani 1 1 d . . . . .
N005 N 0.4714(3) 0.9669(3) 0.7001(3) 0.0346(7) Uani 1 1 d . . . . .
N006 N 0.2533(3) 0.8639(3) 0.5621(3) 0.0373(7) Uani 1 1 d . . . . .
C008 C 0.0960(2) 0.6544(3) 0.3717(2) 0.0327(12) Uani 0.9532(18) 1 d . U P A 1
C00K C 0.1429(2) 0.6007(3) 0.2648(2) 0.0419(9) Uani 0.9532(18) 1 d G . P A 1
H00K H 0.2482 0.5993 0.2317 0.050 Uiso 0.9532(18) 1 calc R . P A 1
C00N C 0.0323(3) 0.5492(3) 0.2075(2) 0.0417(10) Uani 0.9532(18) 1 d G . P A 1
H00N H 0.0636 0.5133 0.1360 0.050 Uiso 0.9532(18) 1 calc R . P A 1
C00E C -0.1251(2) 0.5514(2) 0.2569(2) 0.0349(8) Uani 0.9532(18) 1 d G . P A 1
N003 N -0.17194(19) 0.6050(2) 0.36375(19) 0.0333(7) Uani 0.9532(18) 1 d G . P A
1
C007 C -0.0614(3) 0.6565(2) 0.42111(19) 0.0333(8) Uani 0.9532(18) 1 d G . P A 1
H007 H -0.0927 0.6924 0.4926 0.040 Uiso 0.9532(18) 1 calc R . P A 1
C009 C 0.7337(4) 0.8850(3) 0.7271(3) 0.0358(8) Uani 1 1 d . . . . .
C00A C 0.5192(4) 0.8651(3) 0.6372(3) 0.0329(8) Uani 1 1 d . . . . .
C00B C 0.4122(4) 0.8132(3) 0.5657(3) 0.0314(8) Uani 1 1 d . . . . .
C00C C 0.4766(4) 0.7133(3) 0.5032(4) 0.0369(8) Uani 1 1 d . . . . .
H00C H 0.5872 0.6804 0.5060 0.044 Uiso 1 1 calc R . . . .
C00D C 0.2099(4) 0.7113(3) 0.4348(3) 0.0332(8) Uani 1 1 d . . . . .
C00F C 0.6088(4) 0.9812(3) 0.7582(3) 0.0338(8) Uani 1 1 d . . . . .
C00G C 0.3761(4) 0.6634(3) 0.4372(3) 0.0375(9) Uani 1 1 d . . . . .
H00G H 0.4187 0.5976 0.3940 0.045 Uiso 1 1 calc R . . . .
C00H C 0.1568(4) 0.8133(3) 0.4972(3) 0.0370(8) Uani 1 1 d . . . . .
H00H H 0.0471 0.8492 0.4939 0.044 Uiso 1 1 calc R . . . .
C00I C -0.2575(4) 0.5029(3) 0.2067(3) 0.0342(9) Uani 0.9532(18) 1 d . . P A 1
H00I H -0.3104 0.4488 0.2812 0.041 Uiso 0.9532(18) 1 calc R . P A 1
C00J C 0.8885(4) 0.8732(4) 0.7730(4) 0.0456(10) Uani 1 1 d . . . . .
H00J H 0.9729 0.8102 0.7538 0.055 Uiso 1 1 calc R . . . .
C00L C -0.3147(5) 0.6920(4) 0.0265(4) 0.0518(11) Uani 0.9532(18) 1 d . . P A 1
H00A H -0.2711 0.6402 -0.0345 0.078 Uiso 0.9532(18) 1 calc GR . P A 1
H00B H -0.2310 0.7319 0.0516 0.078 Uiso 0.9532(18) 1 calc GR . P A 1
H00D H -0.4008 0.7609 -0.0137 0.078 Uiso 0.9532(18) 1 calc GR . P A 1
C00M C 0.6336(4) 1.0668(4) 0.8305(4) 0.0441(9) Uani 1 1 d . . . . .
H00M H 0.5500 1.1314 0.8483 0.053 Uiso 1 1 calc R . . . .
C00O C 0.9132(5) 0.9580(4) 0.8479(4) 0.0492(10) Uani 1 1 d . . . . .
H00O H 1.0157 0.9514 0.8803 0.059 Uiso 1 1 calc R . . . .
C00P C -0.2962(5) 0.3512(4) 0.0855(4) 0.0486(11) Uani 0.9532(18) 1 d . . P A 1
H00E H -0.3718 0.4148 0.0267 0.073 Uiso 0.9532(18) 1 calc GR . P A 1
H00F H -0.3536 0.3065 0.1601 0.073 Uiso 0.9532(18) 1 calc GR . P A 1
H00L H -0.2388 0.2867 0.0414 0.073 Uiso 0.9532(18) 1 calc GR . P A 1
C00Q C 0.7872(5) 1.0537(4) 0.8761(4) 0.0489(10) Uani 1 1 d . . . . .
H00Q H 0.8075 1.1096 0.9267 0.059 Uiso 1 1 calc R . . . .
C00R C 0.3150(4) 1.0503(4) 0.7062(4) 0.0479(10) Uani 1 1 d . . . . .
H00P H 0.2613 1.0680 0.6244 0.072 Uiso 1 1 calc GR . . . .
H00R H 0.3299 1.1331 0.7231 0.072 Uiso 1 1 calc GR . . . .
H00S H 0.2503 1.0050 0.7752 0.072 Uiso 1 1 calc GR . . . .
Br0 Br 0.0458(18) 0.6727(11) 0.3276(13) 0.067(5) Uani 0.0468(18) 1 d . U P A 2
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'
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
_geom_angle_publ_flag
C00I O001 C00L 113.8(3) . . ?
C00I O002 C00P 112.2(3) . . ?
C00A N004 C009 105.3(3) . . ?
C00A N005 C00F 106.2(3) . . ?
C00A N005 C00R 130.4(3) . . ?
C00F N005 C00R 123.4(3) . . ?
C00B N006 C00H 117.9(3) . . ?
C00K C008 C007 120.0 . . ?
C00K C008 C00D 121.65(19) . . ?
C007 C008 C00D 118.34(19) . . ?
C00N C00K C008 120.0 . . ?
C00E C00N C00K 120.0 . . ?
C00N C00E N003 120.0 . . ?
C00N C00E C00I 126.89(18) . . ?
N003 C00E C00I 113.10(18) . . ?
C007 N003 C00E 120.0 . . ?
N003 C007 C008 120.0 . . ?
N004 C009 C00F 110.1(3) . . ?
N004 C009 C00J 130.3(3) . . ?
C00J C009 C00F 119.6(3) . . ?
N004 C00A N005 112.7(3) . . ?
N004 C00A C00B 122.0(3) . . ?
N005 C00A C00B 125.2(3) . . ?
N006 C00B C00A 118.9(3) . . ?
N006 C00B C00C 121.6(3) . . ?
C00C C00B C00A 119.5(3) . . ?
C00G C00C C00B 119.5(3) . . ?
C00G C00D C008 121.8(3) . . ?
C00G C00D Br0 127.2(5) . . ?
C00H C00D C008 121.9(3) . . ?
C00H C00D C00G 116.3(3) . . ?
C00H C00D Br0 115.6(5) . . ?
N005 C00F C009 105.7(3) . . ?
C00M C00F N005 131.8(3) . . ?
C00M C00F C009 122.5(3) . . ?
C00C C00G C00D 120.2(3) . . ?
N006 C00H C00D 124.4(3) . . ?
O001 C00I C00E 113.2(2) . . ?
O002 C00I O001 112.5(3) . . ?
O002 C00I C00E 106.2(3) . . ?
C00O C00J C009 117.9(3) . . ?
C00F C00M C00Q 117.3(3) . . ?
C00J C00O C00Q 121.3(3) . . ?
C00M C00Q C00O 121.4(4) . . ?
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
O001 C00I 1.412(4) . ?
O001 C00L 1.428(4) . ?
O002 C00I 1.404(4) . ?
O002 C00P 1.430(4) . ?
N004 C009 1.382(4) . ?
N004 C00A 1.324(4) . ?
N005 C00A 1.383(4) . ?
N005 C00F 1.387(4) . ?
N005 C00R 1.451(4) . ?
N006 C00B 1.344(4) . ?
N006 C00H 1.346(4) . ?
C008 C00K 1.3900 . ?
C008 C007 1.3900 . ?
C008 C00D 1.482(4) . ?
C00K C00N 1.3900 . ?
C00N C00E 1.3900 . ?
C00E N003 1.3900 . ?
C00E C00I 1.478(3) . ?
N003 C007 1.3900 . ?
C009 C00F 1.405(5) . ?
C009 C00J 1.388(5) . ?
C00A C00B 1.462(5) . ?
C00B C00C 1.390(5) . ?
C00C C00G 1.372(5) . ?
C00D C00G 1.396(5) . ?
C00D C00H 1.388(5) . ?
C00D Br0 1.991(13) . ?
C00F C00M 1.366(5) . ?
C00J C00O 1.378(5) . ?
C00M C00Q 1.376(5) . ?
C00O C00Q 1.396(6) . ?
