#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:15:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179834 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013061.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_7013061
loop_
_publ_author_name
'Wu, Chuan-De'
'Lu, Can-Zhong'
'Lu, Shao-Fang'
'Zhuang, Hong-Hui'
'Huang, Jin-Shun'
_publ_section_title
;
 Synthesis, structures and properties of a series of novel left- and
 right-handed metal coordination double helicates with chiral channels
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              3192
_journal_paper_doi               10.1039/b303943a
_journal_year                    2003
_chemical_formula_sum            'C8 H28 Gd Mo2 N O26'
_chemical_formula_weight         903.44
_chemical_name_systematic
;
?
;
_space_group_IT_number           179
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.2980(2)
_cell_length_b                   15.2980(2)
_cell_length_c                   18.6613(3)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.66
_cell_volume                     3782.18(9)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11499
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.692
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8555
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2634
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(1)
_refine_ls_extinction_coef       0.00026(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0288P)²+3.8408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                2038
_reflns_number_total             2253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303943a.txt
_cod_data_source_block           B301542D
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3782.2(1)
_cod_original_sg_symbol_H-M      P6522
_cod_database_code               7013061
#BEGIN Tags that were not found in dictionaries:
_refine_ls_r_factor_ref          0.0333
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.272424(15) -0.45515(3) 0.2500 0.02538(13) Uani 1 2 d S . .
Mo Mo 0.12684(4) -0.72043(4) -0.02144(2) 0.02985(16) Uani 1 1 d . . .
O1 O 0.1708(3) -0.6062(4) 0.0655(2) 0.0360(11) Uani 1 1 d . . .
O2 O 0.2967(3) -0.5036(3) 0.1360(2) 0.0358(11) Uani 1 1 d . . .
O3 O 0.2707(3) -0.6675(3) -0.00734(18) 0.0310(9) Uani 1 1 d . . .
O4 O 0.2979(3) -0.7123(3) 0.13849(19) 0.0339(10) Uani 1 1 d . . .
O5 O 0.5035(3) -0.6212(4) 0.0174(2) 0.0429(12) Uani 1 1 d . . .
O6 O 0.4194(3) -0.7599(3) 0.0827(2) 0.0366(10) Uani 1 1 d . . .
O7 O 0.0709(4) -0.8157(4) 0.0393(2) 0.0463(13) Uani 1 1 d . . .
O8 O 0.1242(4) -0.7803(4) -0.0985(2) 0.0502(13) Uani 1 1 d . . .
O9 O 0.4453(4) -0.3955(5) 0.2752(3) 0.0697(18) Uani 1 1 d . . .
H9A H 0.4805 -0.3455 0.2507 0.084 Uiso 1 1 calc R . .
H9B H 0.4627 -0.4275 0.3078 0.084 Uiso 1 1 d R . .
O10 O 0.2916(6) -0.5982(5) 0.2675(3) 0.087(2) Uani 1 1 d . . .
H10A H 0.3372 -0.5936 0.2418 0.105 Uiso 1 1 calc R . .
H10B H 0.2513 -0.6467 0.2986 0.105 Uiso 1 1 d R . .
O11 O 0.3655(5) -0.3086(4) 0.1735(3) 0.079(2) Uani 1 1 d . . .
H11A H 0.4085 -0.3142 0.1510 0.095 Uiso 1 1 calc R . .
H11B H 0.3491 -0.2597 0.1733 0.095 Uiso 1 1 d R . .
O101 O 0.5625(7) -0.5028(7) -0.0998(4) 0.114(3) Uani 1 1 d . . .
O102 O 0.716(2) -0.1422(10) 0.4167 0.147(11) Uani 0.50 2 d SP . .
O103 O 0.6280(13) -0.2984(14) 0.3773(7) 0.113(6) Uani 0.50 1 d P . .
O104 O 0.0329(11) -0.9836(6) -0.0833 0.25(2) Uani 0.50 2 d SP . .
N1 N 0.2197(5) -0.7803(5) 0.3333 0.051(2) Uani 1 2 d S . .
C1 C 0.2599(5) -0.5661(4) 0.0850(3) 0.0291(14) Uani 1 1 d . . .
C2 C 0.3272(5) -0.5945(5) 0.0452(3) 0.0260(13) Uani 1 1 d . . .
H2A H 0.3810 -0.5344 0.0216 0.031 Uiso 1 1 calc R . .
C3 C 0.3745(5) -0.6353(5) 0.0979(3) 0.0280(14) Uani 1 1 d . . .
H3A H 0.4184 -0.5805 0.1305 0.034 Uiso 1 1 calc R . .
C4 C 0.4381(5) -0.6748(6) 0.0618(3) 0.0353(16) Uani 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'
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'
Mo Mo -1.6832 0.6857 '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'
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
_geom_angle_publ_flag
O2 Gd O2 148.2(2) . 11_655 ?
O2 Gd O10 73.80(17) . . ?
O2 Gd O10 80.88(17) 11_655 . ?
O2 Gd O10 80.88(17) . 11_655 ?
O2 Gd O10 73.80(17) 11_655 11_655 ?
O10 Gd O10 73.9(4) . 11_655 ?
O2 Gd O9 88.82(17) . . ?
O2 Gd O9 101.70(16) 11_655 . ?
O10 Gd O9 72.5(3) . . ?
O10 Gd O9 146.4(2) 11_655 . ?
O2 Gd O9 101.70(16) . 11_655 ?
O2 Gd O9 88.82(17) 11_655 11_655 ?
O10 Gd O9 146.4(2) . 11_655 ?
O10 Gd O9 72.5(3) 11_655 11_655 ?
O9 Gd O9 141.1(3) . 11_655 ?
O2 Gd O11 142.39(16) . 11_655 ?
O2 Gd O11 69.25(16) 11_655 11_655 ?
O10 Gd O11 129.1(2) . 11_655 ?
O10 Gd O11 130.30(19) 11_655 11_655 ?
O9 Gd O11 74.5(2) . 11_655 ?
O9 Gd O11 74.7(2) 11_655 11_655 ?
O2 Gd O11 69.25(16) . . ?
O2 Gd O11 142.39(16) 11_655 . ?
O10 Gd O11 130.30(19) . . ?
O10 Gd O11 129.1(2) 11_655 . ?
O9 Gd O11 74.7(2) . . ?
O9 Gd O11 74.5(2) 11_655 . ?
O11 Gd O11 73.9(3) 11_655 . ?
O8 Mo O7 103.7(2) . . ?
O8 Mo O4 104.3(2) . 6_444 ?
O7 Mo O4 93.5(2) . 6_444 ?
O8 Mo O3 93.2(2) . . ?
O7 Mo O3 104.3(2) . . ?
O4 Mo O3 151.31(18) 6_444 . ?
O8 Mo O6 88.5(2) . 6_444 ?
O7 Mo O6 165.2(2) . 6_444 ?
O4 Mo O6 74.96(16) 6_444 6_444 ?
O3 Mo O6 83.14(16) . 6_444 ?
O8 Mo O1 163.4(2) . . ?
O7 Mo O1 90.7(2) . . ?
O4 Mo O1 82.68(16) 6_444 . ?
O3 Mo O1 74.93(15) . . ?
O6 Mo O1 78.69(16) 6_444 . ?
C1 O1 Mo 115.4(4) . . ?
C1 O2 Gd 147.3(4) . . ?
C2 O3 Mo 122.8(3) . . ?
C3 O4 Mo 123.1(4) . 5_655 ?
C4 O6 Mo 116.4(4) . 5_655 ?
O1 C1 O2 124.0(6) . . ?
O1 C1 C2 117.2(5) . . ?
O2 C1 C2 118.8(6) . . ?
O3 C2 C1 109.6(5) . . ?
O3 C2 C3 110.7(5) . . ?
C1 C2 C3 109.5(5) . . ?
O4 C3 C2 109.0(5) . . ?
O4 C3 C4 109.6(5) . . ?
C2 C3 C4 113.6(5) . . ?
O5 C4 O6 126.0(6) . . ?
O5 C4 C3 119.5(6) . . ?
O6 C4 C3 114.4(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O2 2.343(4) . ?
Gd O2 2.343(4) 11_655 ?
Gd O10 2.372(5) . ?
Gd O10 2.372(5) 11_655 ?
Gd O9 2.374(5) . ?
Gd O9 2.374(5) 11_655 ?
Gd O11 2.430(5) 11_655 ?
Gd O11 2.430(5) . ?
Mo O8 1.695(4) . ?
Mo O7 1.701(4) . ?
Mo O4 1.944(4) 6_444 ?
Mo O3 1.946(4) . ?
Mo O6 2.205(4) 6_444 ?
Mo O1 2.227(4) . ?
O1 C1 1.238(7) . ?
O2 C1 1.264(7) . ?
O3 C2 1.410(7) . ?
O4 C3 1.397(7) . ?
O4 Mo 1.944(4) 5_655 ?
O5 C4 1.241(7) . ?
O6 C4 1.247(8) . ?
O6 Mo 2.205(4) 5_655 ?
C1 C2 1.499(8) . ?
C2 C3 1.527(8) . ?
C3 C4 1.535(9) . ?
