#------------------------------------------------------------------------------
#$Date: 2016-04-05 19:36:20 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181682 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/83/7038362.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_7038362
loop_
_publ_author_name
'Tan, Xiao-Feng'
'Zhou, Jian'
'Fu, Lianshe'
'Xiao, Hong-Ping'
'Zou, Hua-Hong'
'Tang, Qiuling'
_publ_section_title
;
 A series of new lanthanide fumarates displaying three types of 3-D
 frameworks.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5253
_journal_page_last               5261
_journal_paper_doi               10.1039/c6dt00205f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C6 H7 Ho O8'
_chemical_formula_sum            'C6 H7 Ho O8'
_chemical_formula_weight         372.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.566(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4773(10)
_cell_length_b                   8.1182(9)
_cell_length_c                   12.2797(13)
_cell_measurement_reflns_used    1649
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.68
_cell_volume                     944.43(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4920
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    8.400
_exptl_absorpt_correction_T_max  0.2546
_exptl_absorpt_correction_T_min  0.1558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.568
_refine_diff_density_min         -2.365
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1649
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0285
_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)+(0.0413P)²+3.1969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                1570
_reflns_number_total             1649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00205f2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7038358--7038364.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7038362
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ho1 Ho 0.30932(3) 0.05653(3) 0.580854(17) 0.00330(13) Uani 1 1 d .
O1 O 0.5188(4) 0.1684(5) 0.6461(3) 0.0121(9) Uani 1 1 d .
O1W O 0.1081(4) -0.1051(5) 0.6328(3) 0.0118(9) Uani 1 1 d D
O2W O 0.2613(4) 0.1119(5) 0.7646(3) 0.0089(8) Uani 1 1 d D
O2 O 0.7164(4) 0.1437(5) 0.5511(3) 0.0129(9) Uani 1 1 d .
O3 O 1.0797(4) 0.3403(5) 0.8226(3) 0.0085(8) Uani 1 1 d .
O4 O 0.8890(4) 0.3341(5) 0.9235(3) 0.0135(9) Uani 1 1 d .
O5 O 0.2561(5) 0.3519(5) 0.5963(3) 0.0122(9) Uani 1 1 d .
O6 O 0.0975(4) 0.2012(5) 0.5125(3) 0.0138(9) Uani 1 1 d .
C1 C 0.6505(6) 0.1831(7) 0.6350(4) 0.0082(12) Uani 1 1 d .
C2 C 0.7324(6) 0.2499(7) 0.7302(5) 0.0094(12) Uani 1 1 d .
H2 H 0.674(7) 0.292(8) 0.785(5) 0.009(16) Uiso 1 1 d .
C3 C 0.8704(7) 0.2332(7) 0.7423(5) 0.0113(12) Uani 1 1 d .
H3 H 0.928(8) 0.186(9) 0.695(6) 0.03(2) Uiso 1 1 d .
C4 C 0.9503(6) 0.3046(7) 0.8365(4) 0.0072(11) Uani 1 1 d .
C5 C 0.1430(6) 0.3404(7) 0.5406(4) 0.0084(12) Uani 1 1 d .
C6 C 0.0686(7) 0.4972(8) 0.5088(5) 0.0140(12) Uani 1 1 d .
H6A H 0.1212 0.5931 0.5014 0.017 Uiso 1 1 calc R
H2WB H 0.184(4) 0.160(8) 0.782(5) 0.015(18) Uiso 1 1 d D
H1WB H 0.125(8) -0.191(6) 0.672(5) 0.03(2) Uiso 1 1 d D
H2WA H 0.243(8) 0.032(6) 0.808(5) 0.02(2) Uiso 1 1 d D
H1WA H 0.043(7) -0.120(12) 0.584(5) 0.05(3) Uiso 1 1 d 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'
Ho Ho -0.2175 4.6783 '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
O4 Ho1 O2 73.09(15) 4_565 3_656
O4 Ho1 O1 80.74(15) 4_565 .
O2 Ho1 O1 126.58(14) 3_656 .
O4 Ho1 O3 124.48(14) 4_565 2_646
O2 Ho1 O3 82.25(14) 3_656 2_646
O1 Ho1 O3 75.53(14) . 2_646
O4 Ho1 O2W 144.70(15) 4_565 .
O2 Ho1 O2W 142.04(14) 3_656 .
O1 Ho1 O2W 77.24(14) . .
O3 Ho1 O2W 75.81(14) 2_646 .
O4 Ho1 O1W 136.00(14) 4_565 .
O2 Ho1 O1W 74.51(14) 3_656 .
O1 Ho1 O1W 143.18(14) . .
O3 Ho1 O1W 78.84(14) 2_646 .
O2W Ho1 O1W 71.12(14) . .
O4 Ho1 O6 79.04(15) 4_565 .
O2 Ho1 O6 91.55(14) 3_656 .
O1 Ho1 O6 128.21(15) . .
O3 Ho1 O6 151.69(14) 2_646 .
O2W Ho1 O6 93.37(14) . .
O1W Ho1 O6 72.89(14) . .
O4 Ho1 O5 76.02(14) 4_565 .
O2 Ho1 O5 136.43(14) 3_656 .
O1 Ho1 O5 76.44(14) . .
O3 Ho1 O5 141.20(13) 2_646 .
O2W Ho1 O5 72.23(13) . .
O1W Ho1 O5 110.14(15) . .
O6 Ho1 O5 52.56(14) . .
O4 Ho1 C5 74.32(15) 4_565 .
O2 Ho1 C5 113.85(15) 3_656 .
O1 Ho1 C5 102.13(16) . .
O3 Ho1 C5 159.43(14) 2_646 .
O2W Ho1 C5 83.72(14) . .
O1W Ho1 C5 92.78(16) . .
O6 Ho1 C5 26.28(16) . .
O5 Ho1 C5 26.39(15) . .
C1 O1 Ho1 147.4(4) . .
Ho1 O1W H1WB 117(5) . .
Ho1 O1W H1WA 117(6) . .
H1WB O1W H1WA 113(8) . .
Ho1 O2W H2WB 120(5) . .
Ho1 O2W H2WA 120(5) . .
H2WB O2W H2WA 91(7) . .
C1 O2 Ho1 135.1(4) . 3_656
C4 O3 Ho1 121.3(3) . 2_656
C4 O4 Ho1 166.2(4) . 4_666
C5 O5 Ho1 93.4(3) . .
C5 O6 Ho1 93.7(3) . .
O2 C1 O1 125.2(5) . .
O2 C1 C2 118.3(5) . .
O1 C1 C2 116.4(5) . .
C3 C2 C1 123.1(5) . .
C3 C2 H2 124(4) . .
C1 C2 H2 113(4) . .
C2 C3 C4 122.1(5) . .
C2 C3 H3 126(5) . .
C4 C3 H3 112(5) . .
O4 C4 O3 122.8(5) . .
O4 C4 C3 120.0(5) . .
O3 C4 C3 117.1(5) . .
O6 C5 O5 119.9(5) . .
O6 C5 C6 122.4(5) . .
O5 C5 C6 117.7(5) . .
O6 C5 Ho1 60.0(3) . .
O5 C5 Ho1 60.2(3) . .
C6 C5 Ho1 172.6(4) . .
C6 C6 C5 121.9(8) 3_566 .
C6 C6 H6A 119.1 3_566 .
C5 C6 H6A 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O4 2.274(4) 4_565
Ho1 O2 2.303(4) 3_656
Ho1 O1 2.306(4) .
Ho1 O3 2.351(4) 2_646
Ho1 O2W 2.357(4) .
Ho1 O1W 2.415(4) .
Ho1 O6 2.454(4) .
Ho1 O5 2.459(4) .
Ho1 C5 2.828(6) .
O1 C1 1.265(7) .
O1W H1WB 0.859(10) .
O1W H1WA 0.859(10) .
O2W H2WB 0.859(10) .
O2W H2WA 0.861(10) .
O2 C1 1.261(7) .
O2 Ho1 2.303(4) 3_656
O3 C4 1.276(7) .
O3 Ho1 2.351(4) 2_656
O4 C4 1.253(7) .
O4 Ho1 2.274(4) 4_666
O5 C5 1.259(7) .
O6 C5 1.254(7) .
C1 C2 1.488(8) .
C2 C3 1.319(9) .
C2 H2 0.95(6) .
C3 C4 1.483(8) .
C3 H3 0.89(8) .
C5 C6 1.502(9) .
C6 C6 1.313(13) 3_566
C6 H6A 0.9300 .
