#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/72/7217277.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_7217277
loop_
_publ_author_name
'Suman, Kumari'
'Baig, Fayaz'
'Kant, Rajani'
'Gupta, Vivek'
'Mandal, Sanjay'
'Sarkar, Madhushree'
_publ_section_title
;
 Is Metal Metathesis a Framework-Templating Strategy to Synthesize
 Coordination Polymers? Transmetallation Studies involving Flexible
 ligands
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA04166F
_journal_year                    2014
_chemical_formula_moiety         'C32 H40 Cu N8 O6, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C32 H44 Cl2 Cu N8 O16'
_chemical_formula_weight         931.19
_chemical_name_systematic
;
catena-poly[diaquabis-μ-{N, N-bis(3-pyridyl)butanediamido}copper (II) 
perchlorate dihydrate]
 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   11.3423(3)
_cell_length_b                   19.2826(7)
_cell_length_c                   9.5549(3)
_cell_measurement_reflns_used    6996
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.1146
_cell_measurement_theta_min      3.4913
_cell_volume                     2089.74(11)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction,2010)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  PLATON(Spek,2009)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 16.1049
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'omega 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  0.0428
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15254
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.733
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0967P)²+2.9459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.1867
_reflns_number_gt                2989
_reflns_number_total             3675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra04166f2.cif
_cod_data_source_block           CP-3-Cu
_cod_original_sg_symbol_Hall     '-P 2 2ab'
_cod_original_sg_symbol_H-M      'P 21212'
_cod_database_code               7217277
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.6117(5) 0.3808(3) 0.3618(6) 0.0366(14) Uani d . 1
H H1 0.6728 0.3893 0.4244 0.044 Uiso calc R 1
C C2 0.6141(6) 0.3228(4) 0.2810(6) 0.0451(17) Uani d . 1
H H2 0.6758 0.2914 0.2904 0.054 Uiso calc R 1
C C3 0.5256(6) 0.3100(3) 0.1850(6) 0.0401(16) Uani d . 1
H H3 0.5255 0.2696 0.1317 0.048 Uiso calc R 1
C C4 0.4368(5) 0.3593(3) 0.1702(6) 0.0317(13) Uani d . 1
C C5 0.4376(5) 0.4162(3) 0.2567(6) 0.0321(13) Uani d . 1
H H5 0.3776 0.4488 0.2484 0.038 Uiso calc R 1
C C6 0.2818(5) 0.3943(3) 0.0056(8) 0.0329(11) Uani d . 1
C C7 0.1917(6) 0.3665(3) -0.0988(7) 0.0415(15) Uani d . 1
H H7A 0.2145 0.3801 -0.1928 0.05 Uiso calc R 1
H H7B 0.1905 0.3163 -0.0947 0.05 Uiso calc R 1
C C8 0.0693(6) 0.3946(4) -0.0667(7) 0.0412(16) Uani d . 1
H H8A 0.0711 0.4447 -0.0736 0.049 Uiso calc R 1
H H8B 0.0149 0.3776 -0.137 0.049 Uiso calc R 1
C C9 0.0236(5) 0.3747(3) 0.0760(7) 0.0393(16) Uani d . 1
H H9A 0.0744 0.3951 0.1466 0.047 Uiso calc R 1
H H9B 0.0281 0.3247 0.0858 0.047 Uiso calc R 1
C C10 -0.1046(6) 0.3980(3) 0.1041(6) 0.0378(14) Uani d . 1
H H10A -0.1246 0.3882 0.2008 0.045 Uiso calc R 1
H H10B -0.1107 0.4477 0.0901 0.045 Uiso calc R 1
C C11 -0.1901(5) 0.3620(3) 0.0102(7) 0.0321(12) Uani d . 1
C C12 -0.5240(5) 0.3641(3) -0.3528(6) 0.0381(14) Uani d . 1
H H12 -0.5836 0.3564 -0.4178 0.046 Uiso calc R 1
C C13 -0.4903(7) 0.3109(3) -0.2647(7) 0.0450(15) Uani d . 1
H H13 -0.5266 0.2678 -0.2714 0.054 Uiso calc R 1
C C14 -0.4037(6) 0.3217(3) -0.1674(7) 0.0424(16) Uani d . 1
H H14 -0.3787 0.2856 -0.1101 0.051 Uiso calc R 1
C C15 -0.3539(5) 0.3868(3) -0.1556(6) 0.0306(12) Uani d . 1
C C16 -0.3913(5) 0.4376(3) -0.2462(6) 0.0327(13) Uani d . 1
H H16 -0.3588 0.4817 -0.2376 0.039 Uiso calc R 1
Cu Cu1 0.5 0.5 0.50370(10) 0.0310(3) Uani d S 1
N N1 0.5213(5) 0.4261(3) 0.3520(5) 0.0310(12) Uani d . 1
N N2 0.3457(4) 0.3456(2) 0.0740(5) 0.0338(11) Uani d . 1
H H2A 0.3294 0.3028 0.0573 0.041 Uiso calc R 1
N N3 -0.4724(4) 0.4269(3) -0.3467(5) 0.0314(12) Uani d . 1
N N4 -0.2665(4) 0.4045(2) -0.0572(5) 0.0330(11) Uani d . 1
H H4 -0.2609 0.4478 -0.0373 0.04 Uiso calc R 1
O O1 0.2955(4) 0.4560(2) 0.0224(6) 0.0503(12) Uani d . 1
O O2 -0.1925(4) 0.2987(2) -0.0025(6) 0.0455(10) Uani d . 1
Cl Cl1 0.3980(6) 0.1684(5) 0.4364(5) 0.224(4) Uani d . 1
O O4 0.3993(9) 0.1644(5) 0.5735(10) 0.043(2) Uiso d P 0.5
O O6 0.3375(14) 0.2160(15) 0.3459(18) 0.326(14) Uani d . 1
O O5 0.5133(6) 0.1738(4) 0.3973(8) 0.110(3) Uani d . 1
O O3 0.3508(13) 0.1048(10) 0.3950(17) 0.258(10) Uani d . 1
O O1W 0.2846(4) 0.4720(3) 0.5056(8) 0.0706(15) Uani d . 1
H H1WA 0.2662 0.4293 0.4598 0.106 Uiso d R 1
H H1WB 0.2359 0.5057 0.4597 0.106 Uiso d R 1
O O2W 0.2099(10) 0.3429(6) 0.4163(13) 0.143(4) Uani d G 1
H H2WA 0.1351 0.3409 0.414 0.215 Uiso d G 1
H H2WB 0.2362 0.3113 0.4701 0.215 Uiso d G 1
O O4A 0.3490(17) 0.1964(10) 0.567(2) 0.113(6) Uiso d P 0.5
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'
Cu Cu 0.3201 1.2651 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 C2 . . 120.6(6)
N1 C1 H1 . . 119.7
C2 C1 H1 . . 119.7
C1 C2 C3 . . 120.6(6)
C1 C2 H2 . . 119.7
C3 C2 H2 . . 119.7
C2 C3 C4 . . 118.1(6)
C2 C3 H3 . . 121.0
C4 C3 H3 . . 121.0
C5 C4 C3 . . 118.6(5)
C5 C4 N2 . . 123.2(5)
C3 C4 N2 . . 118.0(5)
N1 C5 C4 . . 122.2(5)
N1 C5 H5 . . 118.9
C4 C5 H5 . . 118.9
O1 C6 N2 . . 123.3(6)
O1 C6 C7 . . 121.1(6)
N2 C6 C7 . . 115.6(5)
C8 C7 C6 . . 110.8(5)
C8 C7 H7A . . 109.5
C6 C7 H7A . . 109.5
C8 C7 H7B . . 109.5
C6 C7 H7B . . 109.5
H7A C7 H7B . . 108.1
C9 C8 C7 . . 114.0(5)
C9 C8 H8A . . 108.8
C7 C8 H8A . . 108.8
C9 C8 H8B . . 108.8
C7 C8 H8B . . 108.8
H8A C8 H8B . . 107.7
C8 C9 C10 . . 114.0(5)
C8 C9 H9A . . 108.7
C10 C9 H9A . . 108.7
C8 C9 H9B . . 108.7
C10 C9 H9B . . 108.7
H9A C9 H9B . . 107.6
C11 C10 C9 . . 111.9(5)
C11 C10 H10A . . 109.2
C9 C10 H10A . . 109.2
C11 C10 H10B . . 109.2
C9 C10 H10B . . 109.2
H10A C10 H10B . . 107.9
O2 C11 N4 . . 122.7(6)
O2 C11 C10 . . 122.4(5)
N4 C11 C10 . . 114.9(5)
N3 C12 C13 . . 121.4(6)
N3 C12 H12 . . 119.3
C13 C12 H12 . . 119.3
C14 C13 C12 . . 120.0(6)
C14 C13 H13 . . 120.0
C12 C13 H13 . . 120.0
C13 C14 C15 . . 119.1(6)
C13 C14 H14 . . 120.4
C15 C14 H14 . . 120.4
C16 C15 C14 . . 118.0(6)
C16 C15 N4 . . 117.7(5)
C14 C15 N4 . . 124.3(5)
N3 C16 C15 . . 123.5(6)
N3 C16 H16 . . 118.3
C15 C16 H16 . . 118.3
N3 Cu1 N3 2_566 1_656 90.5(3)
N3 Cu1 N1 2_566 . 177.9(2)
N3 Cu1 N1 1_656 . 89.88(17)
N3 Cu1 N1 2_566 2_665 89.88(17)
N3 Cu1 N1 1_656 2_665 177.9(2)
N1 Cu1 N1 . 2_665 89.8(3)
N3 Cu1 O1W 2_566 . 89.68(19)
N3 Cu1 O1W 1_656 . 89.7(2)
N1 Cu1 O1W . . 88.3(2)
N1 Cu1 O1W 2_665 . 92.3(2)
C5 N1 C1 . . 119.7(5)
C5 N1 Cu1 . . 120.1(4)
C1 N1 Cu1 . . 119.4(4)
C6 N2 C4 . . 125.3(5)
C6 N2 H2A . . 117.4
C4 N2 H2A . . 117.4
C16 N3 C12 . . 117.8(5)
C16 N3 Cu1 . 1_454 120.1(4)
C12 N3 Cu1 . 1_454 121.7(4)
C11 N4 C15 . . 128.4(5)
C11 N4 H4 . . 115.8
C15 N4 H4 . . 115.8
O4 Cl1 O5 . . 105.5(8)
O4 Cl1 O3 . . 103.6(11)
O5 Cl1 O3 . . 111.0(10)
O4 Cl1 O6 . . 130.1(14)
O5 Cl1 O6 . . 104.1(9)
O3 Cl1 O6 . . 102.0(12)
O5 Cl1 O4A . . 124.6(10)
O3 Cl1 O4A . . 114.7(11)
O6 Cl1 O4A . . 95.6(14)
Cu1 O1W H1WA . . 113.3
Cu1 O1W H1WB . . 114.4
H1WA O1W H1WB . . 104.4
H2WA O2W H2WB . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.352(8)
C1 C2 . 1.359(9)
C1 H1 . 0.93
C2 C3 . 1.381(9)
C2 H2 . 0.93
C3 C4 . 1.393(8)
C3 H3 . 0.93
C4 C5 . 1.374(8)
C4 N2 . 1.408(8)
C5 N1 . 1.329(7)
C5 H5 . 0.93
C6 O1 . 1.211(6)
C6 N2 . 1.354(7)
C6 C7 . 1.525(9)
C7 C8 . 1.521(9)
C7 H7A . 0.97
C7 H7B . 0.97
C8 C9 . 1.508(9)
C8 H8A . 0.97
C8 H8B . 0.97
C9 C10 . 1.545(9)
C9 H9A . 0.97
C9 H9B . 0.97
C10 C11 . 1.493(8)
C10 H10A . 0.97
C10 H10B . 0.97
C11 O2 . 1.227(6)
C11 N4 . 1.355(7)
C12 N3 . 1.347(8)
C12 C13 . 1.381(9)
C12 H12 . 0.93
C13 C14 . 1.368(9)
C13 H13 . 0.93
C14 C15 . 1.381(9)
C14 H14 . 0.93
C15 C16 . 1.375(8)
C15 N4 . 1.408(7)
C16 N3 . 1.345(7)
C16 H16 . 0.93
Cu1 N3 2_566 2.031(5)
Cu1 N3 1_656 2.031(5)
Cu1 N1 . 2.046(5)
Cu1 N1 2_665 2.046(5)
Cu1 O1W . 2.502(5)
N2 H2A . 0.86
N3 Cu1 1_454 2.031(5)
N4 H4 . 0.86
Cl1 O4 . 1.312(9)
Cl1 O5 . 1.364(9)
Cl1 O3 . 1.395(13)
Cl1 O6 . 1.436(17)
Cl1 O4A . 1.472(19)
O1W H1WA . 0.9555
O1W H1WB . 0.9599
O2W H2WA . 0.85
O2W H2WB . 0.85
