#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/77/4337776.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_4337776
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            'C21.5 H15.5 Br2 Cl2 Co N10.5 O0.5'
_chemical_formula_weight         718.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 114.9420(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.4329(13)
_cell_length_b                   12.9537(7)
_cell_length_c                   14.6693(7)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.06
_cell_volume                     5071.3(4)
_computing_cell_refinement       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_collection       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XP (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 0.77
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23972
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    4.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Higashi, T. (1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.648
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0362
_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)+(0.0473P)²+8.9158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                4599
_reflns_number_total             5753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402971a_si_002.cif
_cod_data_source_block           1@123K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Empirical'
changed to 'empirical' 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      C2/c
_cod_original_formula_sum        'C21.50 H15.50 Br2 Cl2 Co N10.50 O0.50'
_cod_database_code               4337776
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.372842(13) 0.27605(3) 0.84132(3) 0.02172(10) Uani 1 1 d .
Cl2 Cl 0.28448(3) 0.23930(9) 1.17575(6) 0.0482(3) Uani 1 1 d .
Cl1 Cl 0.60329(3) 0.20763(7) 1.14310(7) 0.0459(2) Uani 1 1 d .
N3 N 0.38547(9) 0.13610(19) 0.82860(19) 0.0261(5) Uani 1 1 d .
N8 N 0.36417(8) 0.41279(18) 0.87720(18) 0.0230(5) Uani 1 1 d .
N4 N 0.44518(8) 0.26726(19) 0.93675(18) 0.0242(5) Uani 1 1 d .
C14 C 0.33655(10) 0.3409(2) 0.9817(2) 0.0249(6) Uani 1 1 d .
N9 N 0.34577(9) 0.43057(19) 0.94729(19) 0.0280(5) Uani 1 1 d .
N2 N 0.43049(9) 0.0924(2) 0.8910(2) 0.0310(6) Uani 1 1 d .
N1 N 0.30395(8) 0.23497(19) 0.71676(18) 0.0232(5) Uani 1 1 d .
N7 N 0.34523(8) 0.24826(19) 0.94638(18) 0.0241(5) Uani 1 1 d .
C1 C 0.26291(11) 0.2859(2) 0.6574(2) 0.0254(6) Uani 1 1 d .
C6 C 0.34976(11) 0.0778(2) 0.7662(2) 0.0309(7) Uani 1 1 d .
H6A H 0.3535 0.0067 0.7632 0.037 Uiso 1 1 calc R
N5 N 0.52624(9) 0.3267(2) 1.0497(2) 0.0334(6) Uani 1 1 d .
C3 C 0.22113(11) 0.1353(3) 0.5704(2) 0.0348(7) Uani 1 1 d .
H3A H 0.1933 0.1024 0.5222 0.042 Uiso 1 1 calc R
N10 N 0.39605(9) 0.3681(2) 0.74036(18) 0.0280(5) Uani 1 1 d .
C13 C 0.37897(10) 0.4914(2) 0.8416(2) 0.0271(6) Uani 1 1 d .
H13A H 0.3769 0.5585 0.8621 0.032 Uiso 1 1 calc R
C15 C 0.31696(11) 0.3399(3) 1.0549(2) 0.0315(7) Uani 1 1 d .
H15A H 0.3098 0.4006 1.0801 0.038 Uiso 1 1 calc R
C10 C 0.51160(11) 0.1451(3) 1.0140(2) 0.0315(7) Uani 1 1 d .
H10A H 0.5239 0.0780 1.0260 0.038 Uiso 1 1 calc R
C9 C 0.54058(11) 0.2272(3) 1.0608(2) 0.0305(7) Uani 1 1 d .
N6 N 0.31794(10) 0.1542(2) 1.0545(2) 0.0361(6) Uani 1 1 d .
C4 C 0.26337(12) 0.0784(3) 0.6296(2) 0.0337(7) Uani 1 1 d .
H4A H 0.2645 0.0075 0.6211 0.040 Uiso 1 1 calc R
C8 C 0.47829(11) 0.3405(2) 0.9880(2) 0.0276(6) Uani 1 1 d .
H8A H 0.4665 0.4080 0.9796 0.033 Uiso 1 1 calc R
C16 C 0.30925(10) 0.2456(3) 1.0865(2) 0.0330(7) Uani 1 1 d .
C11 C 0.41437(12) 0.3454(3) 0.6742(2) 0.0367(8) Uani 1 1 d .
C2 C 0.22057(11) 0.2395(3) 0.5833(2) 0.0313(7) Uani 1 1 d .
H2A H 0.1927 0.2787 0.5437 0.038 Uiso 1 1 calc R
C7 C 0.46156(10) 0.1668(2) 0.9459(2) 0.0265(6) Uani 1 1 d .
C5 C 0.30386(11) 0.1304(2) 0.7017(2) 0.0275(6) Uani 1 1 d .
C17 C 0.33561(11) 0.1621(3) 0.9847(2) 0.0322(7) Uani 1 1 d .
H17A H 0.3420 0.1004 0.9600 0.039 Uiso 1 1 calc R
C12 C 0.39869(10) 0.4696(2) 0.7691(2) 0.0287(6) Uani 1 1 d .
Br1 Br 0.260679(11) 0.43106(2) 0.67169(2) 0.03364(10) Uani 1 1 d .
Br2 Br 0.411114(16) 0.20541(3) 0.63467(3) 0.05129(12) Uani 1 1 d .
C19 C 0.43835(13) 0.5173(3) 0.6633(3) 0.0460(9) Uani 1 1 d .
H19A H 0.4530 0.5666 0.6381 0.055 Uiso 1 1 calc R
C18 C 0.41980(12) 0.5456(3) 0.7316(3) 0.0382(8) Uani 1 1 d .
H18A H 0.4213 0.6139 0.7523 0.046 Uiso 1 1 calc R
C20 C 0.43530(13) 0.4166(3) 0.6323(3) 0.0464(9) Uani 1 1 d .
H20A H 0.4468 0.3967 0.5849 0.056 Uiso 1 1 calc R
N11 N 0.5000 0.1053(3) 1.2500 0.0413(10) Uani 1 2 d S
O1 O 0.5000 0.2782(4) 1.2500 0.099(2) Uani 1 2 d S
C23 C 0.5230(3) 0.1963(6) 1.2899(7) 0.050(2) Uani 0.50 1 d P
C21 C 0.4471(3) 0.0965(9) 1.1823(7) 0.068(3) Uani 0.50 1 d P
C22 C 0.5272(4) 0.0082(7) 1.2912(8) 0.075(3) Uani 0.50 1 d 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'
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
N3 Co1 N8 170.53(11) . .
N3 Co1 N4 79.47(10) . .
N8 Co1 N4 95.01(10) . .
N3 Co1 N7 93.61(11) . .
N8 Co1 N7 79.24(10) . .
N4 Co1 N7 96.10(10) . .
N3 Co1 N1 80.29(10) . .
N8 Co1 N1 106.17(9) . .
N4 Co1 N1 158.00(10) . .
N7 Co1 N1 93.71(9) . .
N3 Co1 N10 108.85(10) . .
N8 Co1 N10 78.38(10) . .
N4 Co1 N10 87.78(9) . .
N7 Co1 N10 157.54(10) . .
N1 Co1 N10 90.64(9) . .
C6 N3 N2 119.6(3) . .
C6 N3 Co1 119.7(2) . .
N2 N3 Co1 120.46(19) . .
C13 N8 N9 118.4(3) . .
C13 N8 Co1 120.9(2) . .
N9 N8 Co1 120.54(18) . .
C8 N4 C7 118.2(2) . .
C8 N4 Co1 131.4(2) . .
C7 N4 Co1 110.41(18) . .
N9 C14 N7 121.0(3) . .
N9 C14 C15 120.4(3) . .
N7 C14 C15 118.5(3) . .
C14 N9 N8 110.2(2) . .
C7 N2 N3 109.0(2) . .
C1 N1 C5 116.4(2) . .
C1 N1 Co1 134.9(2) . .
C5 N1 Co1 108.59(18) . .
C17 N7 C14 117.7(3) . .
C17 N7 Co1 133.2(2) . .
C14 N7 Co1 109.01(19) . .
N1 C1 C2 124.2(3) . .
N1 C1 Br1 119.0(2) . .
C2 C1 Br1 116.8(2) . .
N3 C6 C5 116.0(3) . .
C8 N5 C9 113.6(3) . .
C2 C3 C4 119.9(3) . .
C11 N10 C12 116.7(3) . .
C11 N10 Co1 134.6(2) . .
C12 N10 Co1 107.61(19) . .
N8 C13 C12 116.8(3) . .
C16 C15 C14 116.5(3) . .
C9 C10 C7 116.5(3) . .
N5 C9 C10 126.3(3) . .
N5 C9 Cl1 114.1(2) . .
C10 C9 Cl1 119.5(3) . .
C17 N6 C16 113.3(3) . .
C5 C4 C3 118.2(3) . .
N5 C8 N4 126.8(3) . .
N6 C16 C15 126.3(3) . .
N6 C16 Cl2 115.0(2) . .
C15 C16 Cl2 118.7(3) . .
N10 C11 C20 124.7(4) . .
N10 C11 Br2 116.9(3) . .
C20 C11 Br2 118.4(3) . .
C3 C2 C1 118.3(3) . .
N2 C7 N4 120.0(2) . .
N2 C7 C10 121.6(3) . .
N4 C7 C10 118.4(3) . .
N1 C5 C4 123.0(3) . .
N1 C5 C6 114.9(2) . .
C4 C5 C6 122.2(3) . .
N7 C17 N6 127.6(3) . .
N10 C12 C18 122.1(3) . .
N10 C12 C13 115.3(3) . .
C18 C12 C13 122.6(3) . .
C20 C19 C18 120.2(3) . .
C19 C18 C12 118.6(4) . .
C19 C20 C11 117.7(3) . .
C23 N11 C23 60.1(8) . 2_657
C23 N11 C21 123.7(7) . .
C23 N11 C21 65.2(6) 2_657 .
C23 N11 C21 65.2(6) . 2_657
C23 N11 C21 123.7(7) 2_657 2_657
C21 N11 C21 171.0(10) . 2_657
C23 N11 C22 176.6(6) . 2_657
C23 N11 C22 118.5(6) 2_657 2_657
C21 N11 C22 54.2(6) . 2_657
C21 N11 C22 116.9(8) 2_657 2_657
C23 N11 C22 118.5(6) . .
C23 N11 C22 176.6(6) 2_657 .
C21 N11 C22 116.9(8) . .
C21 N11 C22 54.2(6) 2_657 .
C22 N11 C22 63.2(9) 2_657 .
C23 O1 C23 65.6(8) . 2_657
O1 C23 C23 57.2(4) . 2_657
O1 C23 N11 117.2(7) . .
C23 C23 N11 60.0(4) 2_657 .
O1 C23 C21 167.4(7) . 2_657
C23 C23 C21 118.8(6) 2_657 2_657
N11 C23 C21 60.3(5) . 2_657
C22 C21 N11 63.7(6) 2_657 .
C22 C21 C23 117.2(8) 2_657 2_657
N11 C21 C23 54.5(5) . 2_657
C21 C22 N11 62.1(6) 2_657 .
C21 C22 C22 120.0(6) 2_657 2_657
N11 C22 C22 58.4(5) . 2_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N3 1.876(3) .
Co1 N8 1.895(2) .
Co1 N4 1.998(2) .
Co1 N7 2.055(2) .
Co1 N1 2.147(2) .
Co1 N10 2.222(2) .
Cl2 C16 1.748(3) .
Cl1 C9 1.746(3) .
N3 C6 1.304(4) .
N3 N2 1.375(3) .
N8 C13 1.300(4) .
N8 N9 1.369(3) .
N4 C8 1.340(4) .
N4 C7 1.374(4) .
C14 N9 1.339(4) .
C14 N7 1.373(4) .
C14 C15 1.417(4) .
N2 C7 1.339(4) .
N1 C1 1.329(4) .
N1 C5 1.372(4) .
N7 C17 1.333(4) .
C1 C2 1.398(4) .
C1 Br1 1.896(3) .
C6 C5 1.452(4) .
N5 C8 1.329(4) .
N5 C9 1.345(4) .
C3 C2 1.364(5) .
C3 C4 1.390(5) .
N10 C11 1.326(4) .
N10 C12 1.373(4) .
C13 C12 1.438(4) .
C15 C16 1.358(5) .
C10 C9 1.355(4) .
C10 C7 1.416(4) .
N6 C17 1.333(4) .
N6 C16 1.337(5) .
C4 C5 1.389(4) .
C11 C20 1.389(5) .
C11 Br2 1.894(4) .
C12 C18 1.395(4) .
C19 C20 1.372(6) .
C19 C18 1.378(5) .
N11 C23 1.363(8) .
N11 C23 1.363(8) 2_657
N11 C21 1.455(8) .
N11 C21 1.455(9) 2_657
N11 C22 1.476(9) 2_657
N11 C22 1.476(9) .
O1 C23 1.260(9) .
O1 C23 1.261(9) 2_657
C23 C23 1.365(18) 2_657
C23 C21 1.521(13) 2_657
C21 C22 1.335(14) 2_657
C21 C23 1.521(13) 2_657
C22 C21 1.335(14) 2_657
C22 C22 1.55(2) 2_657
