#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/77/4337778.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_4337778
loop_
_publ_author_name
'Wu, Shu-Qi'
'Wang, Yi-Tong'
'Cui, Ai-Li'
'Kou, Hui-Zhong'
_publ_section_title
;
 Toward Higher Nuclearity: Tetranuclear Cobalt(II) Metallogrid Exhibiting
 Spin Crossover.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2613
_journal_page_last               2618
_journal_paper_doi               10.1021/ic402971a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C64 H44 Br8 Cl4 Co4 N32 O16'
_chemical_formula_weight         2534.02
_space_group_IT_number           137
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2a'
_symmetry_space_group_name_H-M   'P 42/n m c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.615(8)
_cell_length_b                   22.615(8)
_cell_length_c                   13.039(4)
_cell_measurement_reflns_used    16651
_cell_measurement_temperature    253
_cell_measurement_theta_max      29.1095
_cell_measurement_theta_min      2.3841
_cell_volume                     6669(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXTL (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71047
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            42567
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    3.038
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Higashi, T. (1995)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2932
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3090
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1285P)²+5.8215P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2296
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                2566
_reflns_number_total             3090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402971a_si_002.cif
_cod_data_source_block           3@253K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P4(2)/nmc
_cod_database_code               4337778
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z-1/2'
'y, x, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.38755(3) 0.61245(3) 0.2500 0.0740(4) Uani 1 2 d S
Br1 Br 0.50245(4) 0.56697(6) 0.07343(9) 0.1495(6) Uani 1 1 d .
Cl1 Cl 0.5631(2) 0.7500 -0.3504(4) 0.1602(18) Uani 1 2 d S
C1 C 0.5272(3) 0.5972(4) 0.2010(6) 0.105(2) Uani 1 1 d .
C2 C 0.5860(4) 0.6006(5) 0.2204(9) 0.144(4) Uani 1 1 d .
H2A H 0.6133 0.5864 0.1732 0.173 Uiso 1 1 calc R
C3 C 0.6041(3) 0.6251(6) 0.3090(10) 0.162(5) Uani 1 1 d .
H3A H 0.6443 0.6287 0.3230 0.194 Uiso 1 1 calc R
C4 C 0.5624(3) 0.6448(4) 0.3797(8) 0.121(3) Uani 1 1 d .
H4 H 0.5740 0.6615 0.4418 0.145 Uiso 1 1 calc R
C5 C 0.5029(3) 0.6388(3) 0.3543(6) 0.0928(19) Uani 1 1 d .
C6 C 0.4558(3) 0.6573(3) 0.4261(5) 0.0824(16) Uani 1 1 d .
H6A H 0.4637 0.6752 0.4888 0.099 Uiso 1 1 calc R
C7 C 0.3027(3) 0.6485(3) 0.4092(5) 0.0774(15) Uani 1 1 d .
C8 C 0.2500 0.6635(4) 0.4571(6) 0.081(2) Uani 1 2 d S
H8A H 0.2500 0.6831 0.5197 0.097 Uiso 1 2 calc SR
C9 C 0.2500 0.6048(3) 0.2804(7) 0.0721(19) Uani 1 2 d S
H9A H 0.2500 0.5831 0.2199 0.087 Uiso 1 2 calc SR
N1 N 0.4026(2) 0.6466(2) 0.3942(4) 0.0752(12) Uani 1 1 d .
N2 N 0.3557(2) 0.6628(2) 0.4531(4) 0.0849(14) Uani 1 1 d .
H2B H 0.3590 0.6802 0.5115 0.102 Uiso 0.50 1 calc PR
N3 N 0.3023(2) 0.61844(19) 0.3185(4) 0.0737(12) Uani 1 1 d .
N4 N 0.4847(2) 0.6146(2) 0.2642(4) 0.0891(15) Uani 1 1 d .
O1 O 0.5906(7) 0.7500 -0.2589(10) 0.224(7) Uani 1 2 d S
O2 O 0.5303(6) 0.7983(4) -0.3691(11) 0.261(6) Uani 1 1 d .
O3 O 0.6109(13) 0.7500 -0.4215(19) 0.43(2) Uani 1 2 d SU
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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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'
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
N1 Co1 N1 163.0(3) 8_665 .
N1 Co1 N3 75.13(18) 8_665 8_665
N1 Co1 N3 93.07(18) . 8_665
N1 Co1 N3 93.07(19) 8_665 .
N1 Co1 N3 75.13(18) . .
N3 Co1 N3 93.5(2) 8_665 .
N1 Co1 N4 75.6(2) 8_665 8_665
N1 Co1 N4 117.0(2) . 8_665
N3 Co1 N4 150.0(2) 8_665 8_665
N3 Co1 N4 94.53(18) . 8_665
N1 Co1 N4 117.0(2) 8_665 .
N1 Co1 N4 75.6(2) . .
N3 Co1 N4 94.53(18) 8_665 .
N3 Co1 N4 150.0(2) . .
N4 Co1 N4 92.9(3) 8_665 .
O2 Cl1 O2 108.8(10) 13_575 .
O2 Cl1 O1 114.6(7) 13_575 .
O2 Cl1 O1 114.6(7) . .
O2 Cl1 O3 107.6(10) 13_575 .
O2 Cl1 O3 107.6(10) . .
O1 Cl1 O3 103.1(15) . .
N4 C1 C2 125.3(8) . .
N4 C1 Br1 116.1(5) . .
C2 C1 Br1 118.5(7) . .
C3 C2 C1 118.9(9) . .
C3 C2 H2A 120.5 . .
C1 C2 H2A 120.5 . .
C2 C3 C4 119.6(8) . .
C2 C3 H3A 120.2 . .
C4 C3 H3A 120.2 . .
C3 C4 C5 117.8(8) . .
C3 C4 H4 121.1 . .
C5 C4 H4 121.1 . .
N4 C5 C4 122.4(7) . .
N4 C5 C6 116.3(5) . .
C4 C5 C6 121.2(7) . .
N1 C6 C5 114.4(5) . .
N1 C6 H6A 122.8 . .
C5 C6 H6A 122.8 . .
N3 C7 N2 119.2(5) . .
N3 C7 C8 120.3(5) . .
N2 C7 C8 120.4(6) . .
C7 C8 C7 118.4(8) 14_655 .
C7 C8 H8A 120.8 14_655 .
C7 C8 H8A 120.8 . .
N3 C9 N3 127.4(7) . 14_655
N3 C9 H9A 116.3 . .
N3 C9 H9A 116.3 14_655 .
C6 N1 N2 119.5(5) . .
C6 N1 Co1 121.1(4) . .
N2 N1 Co1 119.2(4) . .
N1 N2 C7 112.5(5) . .
N1 N2 H2B 123.8 . .
C7 N2 H2B 123.8 . .
C9 N3 C7 116.7(5) . .
C9 N3 Co1 129.7(4) . .
C7 N3 Co1 112.8(4) . .
C1 N4 C5 115.9(6) . .
C1 N4 Co1 131.6(5) . .
C5 N4 Co1 112.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.061(5) 8_665
Co1 N1 2.061(5) .
Co1 N3 2.130(5) 8_665
Co1 N3 2.130(5) .
Co1 N4 2.205(5) 8_665
Co1 N4 2.205(5) .
Br1 C1 1.884(8) .
Cl1 O2 1.344(9) 13_575
Cl1 O2 1.344(9) .
Cl1 O1 1.345(11) .
Cl1 O3 1.42(2) .
C1 N4 1.326(9) .
C1 C2 1.355(11) .
C2 C3 1.344(13) .
C2 H2A 0.9300 .
C3 C4 1.392(12) .
C3 H3A 0.9300 .
C4 C5 1.394(9) .
C4 H4 0.9300 .
C5 N4 1.361(9) .
C5 C6 1.477(9) .
C6 N1 1.296(8) .
C6 H6A 0.9300 .
C7 N3 1.364(7) .
C7 N2 1.367(7) .
C7 C8 1.388(7) .
C8 C7 1.388(7) 14_655
C8 H8A 0.9300 .
C9 N3 1.319(6) .
C9 N3 1.319(6) 14_655
C9 H9A 0.9300 .
N1 N2 1.360(7) .
N2 H2B 0.8600 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139140871
