#------------------------------------------------------------------------------
#$Date: 2021-01-07 06:37:00 +0200 (Thu, 07 Jan 2021) $
#$Revision: 260626 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/72/7127226.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_7127226
loop_
_publ_author_name
'Rabelo, Renato'
'Toma, Luminita'
'Moliner, Nicolás'
'Julve, Miguel'
'Lloret, Francesc'
'Pasán, Jorge'
'Ruiz-Pérez, Catalina'
'Ruiz-García, Rafael'
'Cano, Joan'
_publ_section_title
;
 Electroswitching of the single-molecule magnet behaviour in an octahedral
 spin crossover cobalt(ii) complex with a redox-active pyridinediimine
 ligand.
;
_journal_issue                   81
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12242
_journal_page_last               12245
_journal_paper_doi               10.1039/d0cc03357j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'18.8(Br3), 5.2(Br5), 8(C42 H38 Co N6 O4), 2(O)'
_chemical_formula_sum            'C336 H304 Br82.4 Co8 N48 O34'
_chemical_formula_weight         12614.28
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-10 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   24.552(5)
_cell_length_b                   24.552(5)
_cell_length_c                   17.693(4)
_cell_measurement_reflns_used    43052
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.856
_cell_measurement_theta_min      2.302
_cell_volume                     10665(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43052
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.856
_diffrn_reflns_theta_max         22.856
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.084
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0799 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.5286.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       prism
_exptl_crystal_F_000             6028
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.577
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0468
_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)+(0.0756P)²+104.7597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3616
_reflns_number_total             3798
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc03357j2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 7127226--7127227.cif.'
_cod_original_cell_volume        10665(5)
_cod_original_formula_sum        'C336 H304 Br82.40 Co8 N48 O34'
_cod_database_code               7127226
_shelx_shelxl_version_number     2018/3
_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. Twinned data refinement
 Scales: 0.93(3)
 0.07(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O2-C21 = O2-C21A
 1.35 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C21A)
5. Rigid body (RIGU) restrains
 O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C21, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Fixed Sof: Br7(0.325) Br8(0.65) Br9(0.65) Br10(0.35) Br11(0.175)
7.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y, -z'
'-x, y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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 -0.21026(8) -0.21026(8) 0.34910(19) 0.0701(8) Uani 1 2 d S T P . .
Br2 Br -0.22730(7) -0.22730(7) 0.20930(19) 0.0662(8) Uani 1 2 d S T P . .
Br3 Br -0.24207(8) -0.24207(8) 0.06766(18) 0.0684(8) Uani 1 2 d S T P . .
Br4 Br -0.10603(8) -0.10603(8) 0.02845(15) 0.0575(7) Uani 1 2 d S T P . .
Br5 Br -0.13932(6) -0.13932(6) -0.09908(14) 0.0460(6) Uani 1 2 d S T P . .
Br6 Br -0.17165(8) -0.17165(8) -0.22765(14) 0.0572(6) Uani 1 2 d S T P . .
Br7 Br 0.000000 -0.500000 0.10808(16) 0.0310(6) Uani 0.65 2 d S T P A 1
Br8 Br 0.10267(9) -0.48780(7) 0.16676(10) 0.0263(4) Uani 0.65 1 d . . . A 1
Br9 Br 0.19503(13) -0.46943(11) 0.20397(13) 0.0360(6) Uani 0.65 1 d . . . A 1
Br10 Br 0.0534(3) -0.49370(19) 0.1727(3) 0.0653(16) Uani 0.35 1 d . . . B 2
Br11 Br 0.1638(6) -0.4777(4) 0.1907(6) 0.045(2) Uani 0.175 1 d . . . B 2
Co1 Co 0.000000 -0.30250(8) 0.000000 0.0198(5) Uani 1 2 d S T P . .
O1 O -0.2478(4) -0.4221(5) 0.0487(6) 0.058(3) Uani 1 1 d . . . . .
O2 O 0.0160(6) -0.1412(8) -0.3195(8) 0.108(6) Uani 1 1 d D U . . .
O3 O 0.000000 0.000000 -0.500000 0.089(12) Uani 1 8 d S T P . .
N1 N -0.0324(4) -0.3562(4) 0.0703(5) 0.023(2) Uani 1 1 d . . . . .
N2 N 0.0554(4) -0.3057(4) 0.0700(5) 0.020(2) Uani 1 1 d . . . . .
N3 N 0.0500(4) -0.2493(4) -0.0474(6) 0.024(2) Uani 1 1 d . . . . .
C1 C -0.0869(5) -0.3759(5) 0.0671(7) 0.024(3) Uani 1 1 d . . . . .
C2 C -0.1237(5) -0.3595(5) 0.1229(7) 0.030(3) Uani 1 1 d . . . . .
H2 H -0.111657 -0.338187 0.164529 0.036 Uiso 1 1 calc R . . . .
C3 C -0.1785(6) -0.3747(6) 0.1167(7) 0.034(3) Uani 1 1 d . . . . .
H3 H -0.204327 -0.362590 0.153060 0.040 Uiso 1 1 calc R . . . .
C4 C -0.1942(6) -0.4066(6) 0.0588(8) 0.042(4) Uani 1 1 d . . . . .
C5 C -0.1580(6) -0.4245(6) 0.0042(8) 0.038(3) Uani 1 1 d . . . . .
H5 H -0.169509 -0.447545 -0.035816 0.046 Uiso 1 1 calc R . . . .
C6 C -0.1049(5) -0.4077(5) 0.0099(7) 0.029(3) Uani 1 1 d . . . . .
H6 H -0.079753 -0.418787 -0.027905 0.035 Uiso 1 1 calc R . . . .
C7 C -0.2862(9) -0.4065(12) 0.0991(15) 0.102(9) Uani 1 1 d . . . . .
H7A H -0.321764 -0.420878 0.083614 0.152 Uiso 1 1 calc R . . . .
H7B H -0.276931 -0.420672 0.149269 0.152 Uiso 1 1 calc R . . . .
H7C H -0.287863 -0.366637 0.101013 0.152 Uiso 1 1 calc R . . . .
C8 C -0.0024(5) -0.3653(5) 0.1298(7) 0.025(3) Uani 1 1 d . . . . .
H8 H -0.013890 -0.388494 0.169732 0.030 Uiso 1 1 calc R . . . .
C9 C 0.0495(5) -0.3378(5) 0.1307(7) 0.023(3) Uani 1 1 d . . . . .
C10 C 0.0928(6) -0.3444(5) 0.1806(8) 0.036(3) Uani 1 1 d . . . . .
H10 H 0.089421 -0.367246 0.223615 0.044 Uiso 1 1 calc R . . . .
C11 C 0.1408(6) -0.3168(5) 0.1661(8) 0.036(3) Uani 1 1 d . . . . .
H11 H 0.170388 -0.319732 0.200492 0.044 Uiso 1 1 calc R . . . .
C12 C 0.1460(6) -0.2853(5) 0.1028(8) 0.039(4) Uani 1 1 d . . . . .
H12 H 0.179810 -0.268201 0.091710 0.047 Uiso 1 1 calc R . . . .
C13 C 0.1022(5) -0.2784(5) 0.0552(7) 0.026(3) Uani 1 1 d . . . . .
C14 C 0.0968(5) -0.2469(5) -0.0139(7) 0.028(3) Uani 1 1 d . . . . .
H14 H 0.125993 -0.225794 -0.033420 0.034 Uiso 1 1 calc R . . . .
C15 C 0.0418(5) -0.2217(6) -0.1180(7) 0.031(3) Uani 1 1 d . . . . .
C16 C -0.0056(6) -0.1951(6) -0.1304(9) 0.047(4) Uani 1 1 d . . . . .
H16 H -0.033125 -0.195026 -0.092695 0.056 Uiso 1 1 calc R . . . .
C17 C -0.0139(7) -0.1680(9) -0.1978(12) 0.078(7) Uani 1 1 d . . . . .
H17 H -0.047516 -0.150087 -0.207196 0.093 Uiso 1 1 calc R . . . .
C18 C 0.0278(9) -0.1672(10) -0.2525(11) 0.079(6) Uani 1 1 d . . . . .
C19 C 0.0759(7) -0.1913(8) -0.2385(10) 0.063(5) Uani 1 1 d . . . . .
H19 H 0.104513 -0.188703 -0.274443 0.076 Uiso 1 1 calc R . . . .
C20 C 0.0841(6) -0.2208(7) -0.1702(8) 0.045(4) Uani 1 1 d . . . . .
H20 H 0.117403 -0.239313 -0.160636 0.054 Uiso 1 1 calc R . . . .
C21 C -0.026(2) -0.107(3) -0.337(3) 0.16(2) Uani 0.45(3) 1 d D U . C 4
H21A H -0.022746 -0.095411 -0.389963 0.233 Uiso 0.45(3) 1 calc R . . C 4
H21B H -0.060734 -0.126166 -0.330122 0.233 Uiso 0.45(3) 1 calc R . . C 4
H21C H -0.024896 -0.075056 -0.304088 0.233 Uiso 0.45(3) 1 calc R . . C 4
C21A C 0.0555(17) -0.146(3) -0.376(2) 0.16(2) Uani 0.55(3) 1 d D U . C 3
H21D H 0.043388 -0.126205 -0.421346 0.233 Uiso 0.55(3) 1 calc R . . C 3
H21E H 0.089929 -0.130474 -0.358296 0.233 Uiso 0.55(3) 1 calc R . . C 3
H21F H 0.060750 -0.184473 -0.388741 0.233 Uiso 0.55(3) 1 calc R . . C 3
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'
Co Co 0.3494 0.9721 '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
Br1 Br2 Br3 178.11(14) . . ?
Br4 Br5 Br6 179.14(14) . . ?
Br8 Br7 Br8 135.52(13) 3_545 . ?
Br9 Br8 Br7 172.38(11) . . ?
Br10 Br10 Br11 173.2(2) 3_545 . ?
N1 Co1 N1 96.5(6) 6 . ?
N2 Co1 N1 95.6(4) 6 . ?
N2 Co1 N1 95.6(4) . 6 ?
N2 Co1 N1 81.1(4) 6 6 ?
N2 Co1 N1 81.1(4) . . ?
N2 Co1 N2 175.1(6) . 6 ?
N2 Co1 N3 81.7(4) . . ?
N2 Co1 N3 81.7(4) 6 6 ?
N2 Co1 N3 101.6(4) . 6 ?
N2 Co1 N3 101.6(4) 6 . ?
N3 Co1 N1 85.6(4) 6 . ?
N3 Co1 N1 162.8(4) 6 6 ?
N3 Co1 N1 162.8(4) . . ?
N3 Co1 N1 85.6(4) . 6 ?
N3 Co1 N3 97.4(6) 6 . ?
C7 O1 C4 120.0(15) . . ?
C18 O2 C21A 116(2) . . ?
C21 O2 C18 130(3) . . ?
C1 N1 Co1 125.4(8) . . ?
C8 N1 Co1 113.3(8) . . ?
C8 N1 C1 120.3(10) . . ?
C9 N2 Co1 119.0(8) . . ?
C9 N2 C13 122.5(10) . . ?
C13 N2 Co1 118.4(8) . . ?
C14 N3 Co1 112.7(8) . . ?
C14 N3 C15 120.2(10) . . ?
C15 N3 Co1 126.4(8) . . ?
C2 C1 N1 118.8(11) . . ?
C6 C1 N1 122.2(11) . . ?
C6 C1 C2 119.0(12) . . ?
C1 C2 C3 119.3(12) . . ?
C4 C3 C2 119.3(13) . . ?
O1 C4 C5 115.7(13) . . ?
C3 C4 O1 122.1(14) . . ?
C3 C4 C5 122.2(13) . . ?
C6 C5 C4 117.6(13) . . ?
C1 C6 C5 122.6(13) . . ?
N1 C8 C9 115.3(11) . . ?
N2 C9 C8 111.2(10) . . ?
N2 C9 C10 119.6(12) . . ?
C10 C9 C8 128.9(12) . . ?
C11 C10 C9 118.5(13) . . ?
C12 C11 C10 120.5(13) . . ?
C11 C12 C13 119.8(14) . . ?
N2 C13 C12 118.9(12) . . ?
N2 C13 C14 110.3(10) . . ?
C12 C13 C14 130.7(12) . . ?
N3 C14 C13 116.3(11) . . ?
C16 C15 N3 119.4(12) . . ?
C16 C15 C20 121.8(13) . . ?
C20 C15 N3 118.7(12) . . ?
C15 C16 C17 120.0(14) . . ?
C16 C17 C18 119.5(16) . . ?
O2 C18 C17 116.4(18) . . ?
C19 C18 O2 123.2(17) . . ?
C19 C18 C17 120.4(17) . . ?
C18 C19 C20 120.4(16) . . ?
C15 C20 C19 117.8(13) . . ?
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 Br2 2.543(5) . ?
Br2 Br3 2.558(5) . ?
Br4 Br5 2.535(4) . ?
Br5 Br6 2.537(4) . ?
Br7 Br8 2.742(2) 3_545 ?
Br7 Br8 2.743(2) . ?
Br8 Br9 2.404(4) . ?
Br10 Br10 2.640(14) 3_545 ?
Br10 Br11 2.757(17) . ?
Co1 N1 1.979(10) . ?
Co1 N1 1.979(10) 6 ?
Co1 N2 1.842(9) 6 ?
Co1 N2 1.842(9) . ?
Co1 N3 1.979(10) 6 ?
Co1 N3 1.979(10) . ?
O1 C4 1.383(17) . ?
O1 C7 1.35(2) . ?
O2 C18 1.38(2) . ?
O2 C21 1.37(3) . ?
O2 C21A 1.40(2) . ?
N1 C1 1.424(16) . ?
N1 C8 1.304(16) . ?
N2 C9 1.340(16) . ?
N2 C13 1.356(16) . ?
N3 C14 1.295(16) . ?
N3 C15 1.434(16) . ?
C1 C2 1.397(19) . ?
C1 C6 1.353(18) . ?
C2 C3 1.401(19) . ?
C3 C4 1.35(2) . ?
C4 C5 1.39(2) . ?
C5 C6 1.370(18) . ?
C8 C9 1.442(18) . ?
C9 C10 1.389(19) . ?
C10 C11 1.38(2) . ?
C11 C12 1.37(2) . ?
C12 C13 1.376(19) . ?
C13 C14 1.453(18) . ?
C15 C16 1.35(2) . ?
C15 C20 1.39(2) . ?
C16 C17 1.38(2) . ?
C17 C18 1.41(3) . ?
C18 C19 1.34(3) . ?
C19 C20 1.42(2) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.93(3)
2 0.07(3)
