#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:22:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180426 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/95/7209583.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_7209583
loop_
_publ_author_name
'Guo, Xiang-Guang'
'Yang, Wen-Bin'
'Wu, Xiao-Yuan'
'Zhang, Qi-Kai'
'Lin, Lang'
'Yu, RongMin'
'Lu, Can-Zhong'
_publ_section_title
;
 Stoichiometry, temperature, solvent, metal-directed syntheses of
 metal--organic frameworks based on flexible V-shaped
 methylenebis(3,5-dimethylpyrazole) and various aromatic dicarboxylate
 acids
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3654
_journal_paper_doi               10.1039/c3ce00048f
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C23 H20 Br3 Cd Co0 Ho0 N4 O6'
_chemical_formula_weight         800.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.340(6)
_cell_angle_beta                 70.388(6)
_cell_angle_gamma                68.920(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1726(6)
_cell_length_b                   11.8494(7)
_cell_length_c                   13.6326(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1385.48(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9436
_diffrn_reflns_theta_full        74.41
_diffrn_reflns_theta_max         74.41
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    11.764
_exptl_absorpt_correction_T_max  0.2547
_exptl_absorpt_correction_T_min  0.2019
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0499
_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)+(0.1026P)²+1.1915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                4910
_reflns_number_total             5433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce00048f.txt
_cod_data_source_block           a6
_cod_original_cell_volume        1385.48(14)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7209583
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cd1 Cd 0.41187(3) 0.68683(3) 0.57534(2) 0.02287(13) Uani 1 1 d .
Br1 Br -0.13769(6) 0.56068(7) 0.83532(5) 0.04834(19) Uani 1 1 d .
Br3 Br 0.46321(11) 0.80179(6) 0.89077(6) 0.0646(3) Uani 1 1 d .
Br2 Br 0.49052(8) 0.13981(7) 0.83501(5) 0.0566(2) Uani 1 1 d .
O6 O 0.3378(4) 0.6387(3) 0.7663(3) 0.0321(8) Uani 1 1 d .
O2 O 0.4188(4) 0.3133(3) 0.5791(3) 0.0355(8) Uani 1 1 d .
O5 O 0.5691(4) 0.6211(4) 0.6988(3) 0.0400(9) Uani 1 1 d .
N26 N 0.3342(5) 0.8888(4) 0.5862(3) 0.0335(9) Uani 1 1 d .
O1 O 0.4684(4) 0.4551(3) 0.6227(3) 0.0338(8) Uani 1 1 d .
O4 O -0.1328(5) 0.4101(4) 1.0647(3) 0.0495(11) Uani 1 1 d .
H4A H -0.1971 0.3926 1.1185 0.074 Uiso 1 1 calc R
N2 N 0.2138(4) 0.7032(4) 0.5226(3) 0.0292(8) Uani 1 1 d .
N1 N 0.2332(5) 0.6376(4) 0.4536(4) 0.0308(9) Uani 1 1 d .
H31 H 0.3160 0.5937 0.4258 0.037 Uiso 1 1 calc R
C6 C 0.4830(6) 0.6263(4) 0.9529(4) 0.0326(11) Uani 1 1 d .
C27 C 0.3106(5) 1.0008(5) 0.5109(4) 0.0278(10) Uani 1 1 d .
N25 N 0.2568(5) 0.9149(4) 0.6814(4) 0.0353(10) Uani 1 1 d .
H25 H 0.2534 0.8592 0.7436 0.042 Uiso 1 1 calc R
C8 C 0.4661(5) 0.6090(4) 0.7761(4) 0.0277(10) Uani 1 1 d .
C14 C 0.2849(5) 0.3599(5) 0.7432(4) 0.0264(9) Uani 1 1 d .
C5 C 0.4856(5) 0.5539(5) 0.8920(4) 0.0284(10) Uani 1 1 d .
C23 C 0.2166(5) 1.0962(4) 0.5577(4) 0.0263(9) Uani 1 1 d .
C15 C 0.1505(5) 0.4474(5) 0.7479(4) 0.0293(10) Uani 1 1 d .
H15 H 0.1337 0.5156 0.6874 0.035 Uiso 1 1 calc R
C29 C 0.0001(5) 0.7253(4) 0.4925(4) 0.0263(9) Uani 1 1 d .
C16 C 0.0395(6) 0.4347(5) 0.8423(4) 0.0312(10) Uani 1 1 d .
C20 C 0.4001(5) 0.3780(4) 0.6392(4) 0.0260(9) Uani 1 1 d .
C7 C 0.5035(6) 0.4264(5) 0.9407(4) 0.0361(11) Uani 1 1 d .
H7 H 0.5065 0.3753 0.9017 0.043 Uiso 1 1 calc R
C33 C 0.0716(5) 0.7578(4) 0.5470(4) 0.0270(9) Uani 1 1 d .
C24 C 0.1856(6) 1.0381(5) 0.6677(4) 0.0338(11) Uani 1 1 d .
C30 C 0.1079(6) 0.6494(5) 0.4338(4) 0.0311(10) Uani 1 1 d .
C11 C 0.0620(6) 0.3324(5) 0.9329(4) 0.0338(11) Uani 1 1 d .
C28 C -0.1600(5) 0.7660(4) 0.4984(4) 0.0311(10) Uani 1 1 d .
H28A H -0.2117 0.7487 0.5741 0.037 Uiso 1 1 calc R
H28B H -0.1805 0.7157 0.4659 0.037 Uiso 1 1 calc R
C34 C 0.0078(6) 0.8373(6) 0.6233(5) 0.0394(12) Uani 1 1 d .
H34A H 0.0662 0.8088 0.6749 0.059 Uiso 1 1 calc R
H34B H -0.0888 0.8305 0.6610 0.059 Uiso 1 1 calc R
H34C H 0.0047 0.9236 0.5833 0.059 Uiso 1 1 calc R
C36 C 0.3846(7) 1.0084(5) 0.3947(5) 0.0410(13) Uani 1 1 d .
H36A H 0.4043 1.0891 0.3585 0.049 Uiso 1 1 calc R
H36B H 0.3231 0.9980 0.3603 0.049 Uiso 1 1 calc R
H36C H 0.4740 0.9430 0.3905 0.049 Uiso 1 1 calc R
C12 C 0.1959(7) 0.2450(5) 0.9282(4) 0.0391(12) Uani 1 1 d .
H12 H 0.2124 0.1761 0.9882 0.047 Uiso 1 1 calc R
C13 C 0.3065(6) 0.2589(5) 0.8345(4) 0.0344(11) Uani 1 1 d .
O3 O -0.0560(8) 0.2043(5) 1.0924(4) 0.087(2) Uani 1 1 d .
C17 C -0.0502(7) 0.3080(6) 1.0385(4) 0.0418(13) Uani 1 1 d .
C35 C 0.1031(7) 0.5857(6) 0.3590(6) 0.0471(14) Uani 1 1 d .
H35A H 0.1311 0.6339 0.2852 0.071 Uiso 1 1 calc R
H35B H 0.0065 0.5796 0.3733 0.071 Uiso 1 1 calc R
H35C H 0.1687 0.5027 0.3707 0.071 Uiso 1 1 calc R
C37 C 0.0934(8) 1.0874(6) 0.7623(5) 0.0543(17) Uani 1 1 d .
H37A H -0.0069 1.1070 0.7629 0.082 Uiso 1 1 calc R
H37B H 0.1156 1.1622 0.7564 0.082 Uiso 1 1 calc R
H37C H 0.1125 1.0246 0.8284 0.082 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O2 Cd1 N26 106.10(15) 2_666 .
O2 Cd1 N2 101.08(15) 2_666 .
N26 Cd1 N2 94.13(15) . .
O2 Cd1 O6 152.23(14) 2_666 .
N26 Cd1 O6 82.85(14) . .
N2 Cd1 O6 104.46(14) . .
O2 Cd1 O5 98.72(13) 2_666 .
N26 Cd1 O5 92.09(15) . .
N2 Cd1 O5 156.68(14) . .
O6 Cd1 O5 54.11(12) . .
O2 Cd1 O1 89.66(13) 2_666 .
N26 Cd1 O1 162.87(14) . .
N2 Cd1 O1 89.24(14) . .
O6 Cd1 O1 80.05(13) . .
O5 Cd1 O1 78.65(14) . .
O2 Cd1 C8 124.90(15) 2_666 .
N26 Cd1 C8 88.44(15) . .
N2 Cd1 C8 131.21(15) . .
O6 Cd1 C8 27.60(14) . .
O5 Cd1 C8 26.55(13) . .
O1 Cd1 C8 76.81(14) . .
C8 O6 Cd1 92.6(3) . .
C20 O2 Cd1 124.4(3) . 2_666
C8 O5 Cd1 90.1(3) . .
C27 N26 N25 104.3(4) . .
C27 N26 Cd1 132.2(3) . .
N25 N26 Cd1 120.5(3) . .
C20 O1 Cd1 135.4(3) . .
C33 N2 N1 105.8(4) . .
C33 N2 Cd1 136.4(3) . .
N1 N2 Cd1 117.6(3) . .
C30 N1 N2 111.7(4) . .
C7 C6 C5 121.7(5) 2_667 .
C7 C6 Br3 118.1(4) 2_667 .
C5 C6 Br3 120.3(4) . .
N26 C27 C23 111.4(4) . .
N26 C27 C36 119.1(5) . .
C23 C27 C36 129.5(4) . .
C24 N25 N26 112.5(4) . .
O5 C8 O6 123.0(4) . .
O5 C8 C5 121.4(4) . .
O6 C8 C5 115.6(4) . .
O5 C8 Cd1 63.4(3) . .
O6 C8 Cd1 59.8(2) . .
C5 C8 Cd1 172.9(3) . .
C15 C14 C13 118.2(4) . .
C15 C14 C20 118.7(4) . .
C13 C14 C20 123.1(4) . .
C7 C5 C6 117.7(4) . .
C7 C5 C8 119.1(5) . .
C6 C5 C8 123.2(4) . .
C24 C23 C27 105.2(4) . .
C24 C23 C28 126.7(5) . 2_576
C27 C23 C28 128.1(5) . 2_576
C14 C15 C16 120.9(5) . .
C30 C29 C33 105.2(4) . .
C30 C29 C28 127.9(5) . .
C33 C29 C28 126.9(5) . .
C11 C16 C15 120.3(5) . .
C11 C16 Br1 123.8(4) . .
C15 C16 Br1 115.8(4) . .
O2 C20 O1 126.7(4) . .
O2 C20 C14 116.4(4) . .
O1 C20 C14 116.8(4) . .
C5 C7 C6 120.7(5) . 2_667
N2 C33 C29 109.8(4) . .
N2 C33 C34 121.5(4) . .
C29 C33 C34 128.6(5) . .
N25 C24 C23 106.6(5) . .
N25 C24 C37 121.3(5) . .
C23 C24 C37 132.1(5) . .
N1 C30 C29 107.4(5) . .
N1 C30 C35 121.2(5) . .
C29 C30 C35 131.4(5) . .
C12 C11 C16 118.8(5) . .
C12 C11 C17 116.3(5) . .
C16 C11 C17 124.9(5) . .
C29 C28 C23 113.9(4) . 2_576
C11 C12 C13 120.7(5) . .
C14 C13 C12 121.0(5) . .
C14 C13 Br2 120.2(4) . .
C12 C13 Br2 118.7(4) . .
O3 C17 O4 124.7(5) . .
O3 C17 C11 121.9(6) . .
O4 C17 C11 113.3(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O2 2.228(4) 2_666
Cd1 N26 2.279(4) .
Cd1 N2 2.281(4) .
Cd1 O6 2.359(3) .
Cd1 O5 2.437(4) .
Cd1 O1 2.468(4) .
Cd1 C8 2.726(4) .
Br1 C16 1.887(5) .
Br3 C6 1.897(5) .
Br2 C13 1.897(5) .
O6 C8 1.264(6) .
O2 C20 1.245(6) .
O2 Cd1 2.228(3) 2_666
O5 C8 1.219(6) .
N26 C27 1.343(6) .
N26 N25 1.354(6) .
O1 C20 1.253(6) .
O4 C17 1.297(7) .
N2 C33 1.335(6) .
N2 N1 1.354(6) .
N1 C30 1.339(7) .
C6 C7 1.384(7) 2_667
C6 C5 1.385(7) .
C27 C23 1.395(7) .
C27 C36 1.492(7) .
N25 C24 1.349(6) .
C8 C5 1.522(6) .
C14 C15 1.386(7) .
C14 C13 1.388(7) .
C14 C20 1.506(6) .
C5 C7 1.378(7) .
C23 C24 1.378(7) .
C23 C28 1.511(6) 2_576
C15 C16 1.399(7) .
C29 C30 1.372(7) .
C29 C33 1.417(7) .
C29 C28 1.505(7) .
C16 C11 1.391(7) .
C7 C6 1.384(7) 2_667
C33 C34 1.490(7) .
C24 C37 1.495(8) .
C30 C35 1.497(8) .
C11 C12 1.381(8) .
C11 C17 1.512(7) .
C28 C23 1.511(6) 2_576
C12 C13 1.392(7) .
O3 C17 1.188(8) .
