#------------------------------------------------------------------------------
#$Date: 2016-02-05 02:47:58 +0200 (Fri, 05 Feb 2016) $
#$Revision: 176117 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/72/7037239.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_7037239
loop_
_publ_author_name
'Shi, Jinbiao'
'Zhang, Yan'
'Zhang, Bin'
'Zhu, Daoben'
_publ_section_title
;
 Crystal-to-crystal transformation from a chain compound to a layered
 coordination polymer.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              89
_journal_page_last               92
_journal_paper_doi               10.1039/c5dt03985a
_journal_volume                  45
_journal_year                    2015
_chemical_formula_sum            'C8 H20 Br2 Cu O6'
_chemical_formula_weight         435.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-04 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                103.643(3)
_cell_angle_beta                 101.225(3)
_cell_angle_gamma                101.936(5)
_cell_formula_units_Z            1
_cell_length_a                   5.5714(17)
_cell_length_b                   6.978(2)
_cell_length_c                   10.303(3)
_cell_measurement_reflns_used    1708
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.9947
_cell_measurement_theta_min      3.9011
_cell_volume                     368.14(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_laue_measured_fraction_full 0.980
_diffrn_reflns_laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4709
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.867
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    6.921
_exptl_absorpt_correction_T_max  0.5237
_exptl_absorpt_correction_T_min  0.3196
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       block
_exptl_crystal_F_000             215
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0282P)²+0.1651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1613
_reflns_number_total             1662
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt03985a2.cif
_cod_data_source_block           122
_cod_depositor_comments
'Adding full bibliography for 7037239--7037240.cif.'
_cod_original_cell_volume        368.2(2)
_cod_database_code               7037239
_audit_block_doi                 10.5517/cc1jbsf2
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.290
_shelx_estimated_absorpt_t_max   0.519
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.5000 0.5000 0.01886(10) Uani 1 2 d S P
Br1 Br 0.74450(3) 0.50855(3) 0.72381(2) 0.02251(9) Uani 1 1 d . .
O1 O 0.1132(3) 0.2015(2) 0.49767(14) 0.0200(3) Uani 1 1 d . .
O2 O 0.3368(3) 0.6937(2) 0.58901(18) 0.0265(3) Uani 1 1 d . .
O3 O 0.4208(3) 0.8941(3) 0.85809(16) 0.0327(4) Uani 1 1 d . .
C1 C 0.0879(4) 0.0238(3) 0.3852(2) 0.0218(4) Uani 1 1 d . .
C2 C 0.1371(4) 0.1457(3) 0.6243(2) 0.0210(4) Uani 1 1 d . .
C3 C 0.3963(5) 0.7892(4) 0.9610(2) 0.0343(5) Uani 1 1 d . .
C4 C 0.6354(5) 1.0699(4) 0.9130(2) 0.0320(5) Uani 1 1 d . .
H1 H 0.247(5) -0.030(4) 0.401(3) 0.031(7) Uiso 1 1 d . .
H2 H 0.060(5) 0.064(4) 0.307(3) 0.026(6) Uiso 1 1 d . .
H3 H 0.143(5) 0.262(4) 0.692(3) 0.025(6) Uiso 1 1 d . .
H4 H 0.286(5) 0.106(4) 0.641(3) 0.021(6) Uiso 1 1 d . .
H5 H 0.250(6) 0.673(5) 0.921(3) 0.042(8) Uiso 1 1 d . .
H6 H 0.549(5) 0.740(4) 0.984(3) 0.032(7) Uiso 1 1 d . .
H7 H 0.797(6) 1.028(5) 0.933(3) 0.049(9) Uiso 1 1 d . .
H8 H 0.641(5) 1.140(4) 0.842(3) 0.036(7) Uiso 1 1 d . .
H9 H 0.207(7) 0.691(5) 0.559(4) 0.048(10) Uiso 1 1 d . .
H10 H 0.367(6) 0.729(5) 0.669(4) 0.045(9) Uiso 1 1 d . .
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'
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'
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
O2 Cu1 O2 180.0 2_666 .
O2 Cu1 Br1 90.05(6) 2_666 .
O2 Cu1 Br1 89.95(6) . .
O2 Cu1 Br1 89.95(6) 2_666 2_666
O2 Cu1 Br1 90.05(6) . 2_666
Br1 Cu1 Br1 180.0 . 2_666
C2 O1 C1 109.23(15) . .
Cu1 O2 H9 121(3) . .
Cu1 O2 H10 119(2) . .
H9 O2 H10 110(4) . .
C4 O3 C3 109.50(18) . .
O1 C1 C2 110.59(16) . 2_556
O1 C1 H1 110.4(15) . .
C2 C1 H1 107.7(15) 2_556 .
O1 C1 H2 105.6(17) . .
C2 C1 H2 108.8(16) 2_556 .
H1 C1 H2 114(2) . .
O1 C2 C1 110.96(17) . 2_556
O1 C2 H3 106.1(17) . .
C1 C2 H3 109.6(16) 2_556 .
O1 C2 H4 107.4(16) . .
C1 C2 H4 111.1(16) 2_556 .
H3 C2 H4 112(2) . .
O3 C3 C4 109.9(2) . 2_677
O3 C3 H5 107.0(18) . .
C4 C3 H5 111.2(18) 2_677 .
O3 C3 H6 109.0(17) . .
C4 C3 H6 110.6(17) 2_677 .
H5 C3 H6 109(2) . .
O3 C4 C3 110.2(2) . 2_677
O3 C4 H7 110.9(19) . .
C3 C4 H7 111.4(19) 2_677 .
O3 C4 H8 107.1(17) . .
C3 C4 H8 109.1(17) 2_677 .
H7 C4 H8 108(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9347(16) 2_666
Cu1 O2 1.9348(16) .
Cu1 Br1 2.4198(6) .
Cu1 Br1 2.4198(6) 2_666
O1 C2 1.437(2) .
O1 C1 1.444(2) .
O2 H9 0.73(4) .
O2 H10 0.77(4) .
O3 C4 1.434(3) .
O3 C3 1.435(3) .
C1 C2 1.504(3) 2_556
C1 H1 1.03(3) .
C1 H2 0.91(3) .
C2 C1 1.504(3) 2_556
C2 H3 0.93(3) .
C2 H4 0.92(3) .
C3 C4 1.498(3) 2_677
C3 H5 0.96(3) .
C3 H6 0.99(3) .
C4 C3 1.498(3) 2_677
C4 H7 1.00(3) .
C4 H8 0.97(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H9 O1 0.73(4) 2.10(4) 2.795(2) 159(4) 2_566
O2 H10 O3 0.77(4) 1.95(4) 2.694(2) 162(3) .
C1 H2 Br1 0.91(3) 3.07(3) 3.696(2) 128(2) 2_666
C2 H3 Br1 0.93(3) 3.10(3) 3.766(2) 130(2) 1_455
C4 H8 Br1 0.97(3) 3.10(3) 4.005(3) 157(2) 1_565
