#------------------------------------------------------------------------------
#$Date: 2019-10-24 05:21:48 +0300 (Thu, 24 Oct 2019) $
#$Revision: 219477 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/89/7058902.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_7058902
loop_
_publ_author_name
'Zheng, Teng-Fei'
'Tian, Xue-Mei'
'Wu, Lin-Hui'
'Liu, Sui-Jun'
'Yao, Shu-Li'
'He, Kun-Huan'
'Huang, Hai-Ping'
'Liao, Jinsheng'
'Chen, Jing-Lin'
'Wen, He-Rui'
_publ_section_title
;
 Two GdIII complexes with different structures and magnetocaloric
 properties induced by metal ion sources
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C9NJ04984C
_journal_year                    2019
_chemical_formula_moiety         'C5 H6 Gd O8, 2(H2 O)'
_chemical_formula_sum            'C5 H10 Gd O10'
_chemical_formula_weight         387.38
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-21 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                96.583(2)
_cell_angle_beta                 97.241(2)
_cell_angle_gamma                95.907(2)
_cell_formula_units_Z            2
_cell_length_a                   6.0605(4)
_cell_length_b                   7.7412(5)
_cell_length_c                   10.4334(7)
_cell_measurement_reflns_used    5277
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.11
_cell_volume                     478.95(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      298.82
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6360
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         3.113
_exptl_absorpt_coefficient_mu    6.969
_exptl_absorpt_correction_T_max  0.442
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2191
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0155P)²+0.8081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2092
_reflns_number_total             2191
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj04984c2.cif
_cod_data_source_block           2
_cod_database_code               7058902
_shelx_shelxl_version_number     2017/1
_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_max   0.442
_shelx_estimated_absorpt_t_min   0.275
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C2-H3
 1.896473 with sigma of 0.02
 Gd1-H3
 3.111192 with sigma of 0.02
3.a Free rotating group:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB)
3.b Rotating group:
 O1W(H1WA,H1WB)
3.c Ternary CH refined with riding coordinates:
 C2(H2)
3.d Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
O4 O 0.3847(4) 1.3429(3) 0.9628(2) 0.0218(4) Uani 1 1 d .
O5 O 0.3239(4) 1.2645(3) 0.7534(2) 0.0231(5) Uani 1 1 d .
C4 C 0.3075(5) 1.2302(4) 0.8661(3) 0.0153(5) Uani 1 1 d .
O7 O 0.3163(4) 0.5711(4) 0.3814(2) 0.0332(6) Uani 1 1 d .
O2 O -0.1326(3) 0.7511(3) 0.8080(2) 0.0223(5) Uani 1 1 d .
Gd1 Gd 0.53176(2) 0.56023(2) 0.80598(2) 0.01324(5) Uani 1 1 d D
O1 O 0.1650(3) 0.6102(3) 0.8430(2) 0.0200(4) Uani 1 1 d .
O3 O 0.4504(3) 0.8681(3) 0.8098(2) 0.0205(4) Uani 1 1 d D
H3 H 0.520(3) 0.942(3) 0.768(3) 0.031 Uiso 1 1 d DR
O6 O 0.3330(4) 0.6080(4) 0.5979(2) 0.0331(6) Uani 1 1 d .
O1W O 0.8177(4) 0.3731(3) 0.8689(3) 0.0325(6) Uani 1 1 d .
H1WA H 0.794142 0.274632 0.818718 0.049 Uiso 1 1 d GR
H1WB H 0.803985 0.344146 0.945165 0.049 Uiso 1 1 d GR
C1 C 0.0726(5) 0.7430(4) 0.8161(3) 0.0159(5) Uani 1 1 d .
C2 C 0.2225(5) 0.9049(4) 0.7929(3) 0.0172(6) Uani 1 1 d D
H2 H 0.181023 0.931851 0.704212 0.021 Uiso 1 1 calc R
C5 C 0.3985(6) 0.5510(4) 0.4938(3) 0.0248(7) Uani 1 1 d .
O3W O 0.0867(7) 0.2102(5) 0.4964(3) 0.0616(9) Uani 1 1 d .
H3WA H 0.129978 0.222524 0.577964 0.092 Uiso 1 1 d G
H3WB H -0.011874 0.279991 0.487028 0.092 Uiso 1 1 d G
O2W O 0.6625(7) 0.0245(5) 0.6372(5) 0.0772(13) Uani 1 1 d .
H2WA H 0.681895 0.131328 0.624938 0.116 Uiso 1 1 d G
H2WB H 0.735744 -0.035457 0.587893 0.116 Uiso 1 1 d G
C3 C 0.1920(5) 1.0577(4) 0.8903(3) 0.0217(6) Uani 1 1 d .
H3A H 0.033096 1.066644 0.888008 0.026 Uiso 1 1 calc R
H3B H 0.249318 1.034640 0.976982 0.026 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 0.0033 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'
Gd Gd -0.1653 3.9035 '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'
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
C4 O4 Gd1 152.7(2) . 2_677
C4 O4 Gd1 90.41(17) . 1_565
Gd1 O4 Gd1 116.80(8) 2_677 1_565
C4 O5 Gd1 99.39(18) . 1_565
O4 C4 Gd1 64.15(15) . 1_565
O4 C4 C3 118.5(3) . .
O5 C4 O4 119.9(3) . .
O5 C4 Gd1 55.82(15) . 1_565
O5 C4 C3 121.6(3) . .
C3 C4 Gd1 177.3(2) . 1_565
C5 O7 Gd1 120.1(2) . 2_666
C1 O2 Gd1 138.6(2) . 1_455
O4 Gd1 O4 63.20(8) 2_677 1_545
O4 Gd1 O5 113.40(7) 2_677 1_545
O4 Gd1 C4 25.44(7) 1_545 1_545
O4 Gd1 C4 88.62(8) 2_677 1_545
O4 Gd1 O7 143.84(8) 2_677 2_666
O4 Gd1 O3 80.07(7) 2_677 .
O4 Gd1 O6 146.60(8) 2_677 .
O4 Gd1 O1W 79.34(8) 2_677 .
O5 Gd1 O4 50.22(7) 1_545 1_545
O5 Gd1 C4 24.79(8) 1_545 1_545
O5 Gd1 O3 137.85(7) 1_545 .
O7 Gd1 O4 116.24(8) 2_666 1_545
O7 Gd1 O5 75.46(8) 2_666 1_545
O7 Gd1 C4 95.53(9) 2_666 1_545
O7 Gd1 O3 117.92(8) 2_666 .
O7 Gd1 O6 66.21(8) 2_666 .
O7 Gd1 O1W 68.20(9) 2_666 .
O2 Gd1 O4 135.11(7) 1_655 1_545
O2 Gd1 O4 80.75(8) 1_655 2_677
O2 Gd1 O5 149.13(7) 1_655 1_545
O2 Gd1 C4 149.59(7) 1_655 1_545
O2 Gd1 O7 77.68(9) 1_655 2_666
O2 Gd1 O3 69.47(7) 1_655 .
O2 Gd1 O6 99.11(9) 1_655 .
O2 Gd1 O1W 78.55(8) 1_655 .
O1 Gd1 O4 70.23(7) . 1_545
O1 Gd1 O4 82.38(7) . 2_677
O1 Gd1 O5 77.50(7) . 1_545
O1 Gd1 C4 72.66(7) . 1_545
O1 Gd1 O7 133.10(8) . 2_666
O1 Gd1 O2 132.95(7) . 1_655
O1 Gd1 O3 64.50(7) . .
O1 Gd1 O6 73.39(8) . .
O1 Gd1 O1W 139.87(7) . .
O3 Gd1 O4 124.41(7) . 1_545
O3 Gd1 C4 136.70(7) . 1_545
O6 Gd1 O4 125.75(8) . 1_545
O6 Gd1 O5 83.74(8) . 1_545
O6 Gd1 C4 105.18(9) . 1_545
O6 Gd1 O3 68.97(8) . .
O6 Gd1 O1W 133.69(9) . .
O1W Gd1 O4 69.64(7) . 1_545
O1W Gd1 O5 77.56(8) . 1_545
O1W Gd1 C4 71.48(8) . 1_545
O1W Gd1 O3 144.21(8) . .
C1 O1 Gd1 124.85(18) . .
C2 O3 Gd1 119.49(16) . .
C5 O6 Gd1 120.1(2) . .
O2 C1 O1 124.1(3) . .
O2 C1 C2 117.9(3) . .
O1 C1 C2 118.0(2) . .
O3 C2 C1 108.4(2) . .
O3 C2 C3 110.3(2) . .
C3 C2 C1 108.8(2) . .
O7 C5 O6 126.4(3) . .
O7 C5 C5 117.0(3) . 2_666
O6 C5 C5 116.6(4) . 2_666
C4 C3 C2 113.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4 C4 1.262(4) .
O4 Gd1 2.645(2) 1_565
O4 Gd1 2.416(2) 2_677
O5 C4 1.249(4) .
O5 Gd1 2.464(2) 1_565
C4 Gd1 2.939(3) 1_565
C4 C3 1.506(4) .
O7 Gd1 2.428(2) 2_666
O7 C5 1.249(4) .
O2 Gd1 2.384(2) 1_455
O2 C1 1.244(3) .
Gd1 O1 2.366(2) .
Gd1 O3 2.480(2) .
Gd1 O6 2.433(2) .
Gd1 O1W 2.445(2) .
O1 C1 1.263(3) .
O3 C2 1.432(3) .
O6 C5 1.251(4) .
C1 C2 1.531(4) .
C2 C3 1.511(4) .
C5 C5 1.528(7) 2_666
