A unique μ8-silicate-bridged octametallic [Dy8SiO4] complex exhibiting slow magnetic relaxation
She, Shi-Xiong; Zaworotko, Michael J.; Liu, Wei; Zhang, Zhu-Xiu; Li, Yahong; CrystEngComm 15 (2013) 5003–; doi:10.1039/c3ce40295a

data_7210163
_publ_section_title
;
 A unique \m8-silicate-bridged octametallic [Dy8SiO4] complex exhibiting
 slow magnetic relaxation
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              5003
_journal_paper_doi               10.1039/c3ce40295a
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C148 H108 Dy8 N12 O44 Si'
_chemical_formula_sum            'C148 H108 Dy8 N12 O44 Si'
_chemical_formula_weight         4086.55
_chemical_name_systematic
;
?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-23
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.2454(5)
_cell_length_b                   16.2454(5)
_cell_length_c                   26.0964(9)
_cell_measurement_reflns_used    2315
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.97
_cell_measurement_theta_min      3.2
_cell_volume                     6887.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1384
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42130
_diffrn_reflns_theta_full        66.22
_diffrn_reflns_theta_max         66.22
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.621
_exptl_absorpt_correction_T_max  0.2538
_exptl_absorpt_correction_T_min  0.0881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3948
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5988
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0457
_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/[\s^2^(Fo^2^)+(0.0000P)^2^+1.5308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                4887
_reflns_number_total             5988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40295a.txt
_cod_data_source_block           t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7210163
_olex2_refinement_description
;
1. Others
Fixed U12: Si1(0)
Fixed U13: Si1(0)
Fixed U23: Si1(0)
Fixed Uiso: H1A(0.104) H1B(0.104) H1C(0.104) H3(0.075) H3A(0.1) H3B(0.1)
H4(0.086) H5(0.072) H8(0.057) H10(0.058) H11(0.073) H12(0.081) H13(0.066)
H16A(0.1) H16B(0.1) H16C(0.1) H18(0.067) H19(0.079) H20(0.066) H23(0.054)
H25(0.057) H26(0.073) H27(0.077) H28(0.068) H33(0.069) H34(0.069) H35(0.069)
Fixed X: Si1(0.5) H1A(0.4711) H1B(0.553) H1C(0.5053) H3(0.6555) H3A(0.7984)
H3B(0.8661) H4(0.779) H5(0.8315) H8(0.8347) H10(0.827) H11(0.9239) H12(0.9515)
H13(0.8986) H16A(0.5034) H16B(0.5402) H16C(0.5873) H18(0.4898) H19(0.5287)
H20(0.5902) H23(0.6221) H25(0.7388) H26(0.7877) H27(0.7504) H28(0.6496)
H33(0.6237) H34(0.6913) H35(0.8088)
Fixed Y: Si1(0.5) H1A(0.115) H1B(0.0641) H1C(0.0812) H3(0.0488) H3A(0.7217)
H3B(0.7784) H4(0.0534) H5(0.1758) H8(0.3181) H10(0.4033) H11(0.5009)
H12(0.6143) H13(0.6276) H16A(0.1532) H16B(0.2405) H16C(0.1795) H18(0.2518)
H19(0.3627) H20(0.4736) H23(0.5537) H25(0.6119) H26(0.745) H27(0.8235)
H28(0.7785) H33(0.8886) H34(1.0118) H35(1.0267)
Fixed Z: Si1(0.5) H1A(0.4697) H1B(0.4687) H1C(0.4176) H3(0.4162) H3A(0.4489)
H3B(0.4337) H4(0.3705) H5(0.3436) H8(0.3413) H10(0.2658) H11(0.2371)
H12(0.2857) H13(0.3667) H16A(0.3203) H16B(0.3319) H16C(0.2957) H18(0.1694)
H19(0.1201) H20(0.1573) H23(0.2264) H25(0.245) H26(0.2533) H27(0.3226)
H28(0.3772) H33(0.543) H34(0.5428) H35(0.4979)
;