Flexible linkers and dinuclear metallic nodes build up an original metal‒organic framework
Vlad, Angelica; Zaltariov, Mirela-Fernanda; Shova, Sergiu; Novitchi, Ghenadie; Varganici, Cristian-Dragos; Train, Cyrille; Cazacu, Maria; CrystEngComm 15 (2013) 5368–; doi:10.1039/c3ce40506k

data_7209943
_publ_section_title
;
 Flexible linkers and dinuclear metallic nodes build up an original
 metal--organic framework
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5368
_journal_paper_doi               10.1039/c3ce40506k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety
'0.5(C72 H128 Cu4 N16 O20 Si8), C12 H26 O5 Si2'
_chemical_formula_sum            'C48 H90 Cu2 N8 O15 Si6'
_chemical_formula_weight         1314.90
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-14
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.896(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.423(5)
_cell_length_b                   10.0020(10)
_cell_length_c                   16.5770(18)
_cell_measurement_reflns_used    3193
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1834
_cell_measurement_theta_min      2.3928
_cell_volume                     7131.4(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega -21.00 11.25 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- -17.0127 -99.0000 120.0000 43

2 omega -74.00 -36.50 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- -17.0127 -178.0000 120.0000 50

3 omega -25.00 3.50 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- -17.0127 -99.0000 60.0000 38

4 omega -6.00 76.50 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- 19.6690 38.0000 0.0000 110

5 omega 36.00 95.25 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- 19.6690 178.0000 -150.0000 79

6 omega -53.00 42.25 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- 19.6690 -38.0000 0.0000 127

7 omega -53.00 29.50 0.7500 60.0000
omega____ theta____ kappa____ phi______ frames
- 19.6690 -19.0000 -120.0000 110
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0145998000
_diffrn_orient_matrix_UB_12      -0.0327741000
_diffrn_orient_matrix_UB_13      0.0070348000
_diffrn_orient_matrix_UB_21      0.0049693000
_diffrn_orient_matrix_UB_22      0.0357932000
_diffrn_orient_matrix_UB_23      -0.0328195000
_diffrn_orient_matrix_UB_31      0.0058186000
_diffrn_orient_matrix_UB_32      0.0517755000
_diffrn_orient_matrix_UB_33      0.0271769000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25327
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.0951
_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/[\s^2^(Fo^2^)+(0.1349P)^2^+3.3947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2736
_reflns_number_gt                3358
_reflns_number_total             6251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40506k.txt
_cod_data_source_block           an_1368_av
_cod_original_cell_volume        7131.3(14)
_cod_database_code               7209943
_chemical_oxdiff_formula         'C15 H15 O5 Si2 N2 Cu Cl2'
_chemical_oxdiff_usercomment     AV_115_reluare
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
{H8A,H8B} of C8, {H9A,H9B} of C9, {H10A,H10B} of C10, H2A of C2, H3 of C3,
H4A of C4, H5 of C5, H6 of C6, H1 of C1, H2 of N2, {H15A,H15B} of C15, {H15C,
H15D} of C15X, {H16A,H16B} of C16, {H16C,H16D} of C16X, {H17C,H17D,H17A,H17B}
of C17, {H20A,H20B,H20C,H20D} of C20, {H21A,H21B} of C21, {H21C,H21D} of C21X,
{H22A,H22B} of C22, {H22C,H22D} of C22X
At 1.5 times of:
{H11A,H11B,H11C} of C11, H4 of N4, H7 of O7, {H12A,H12B,H12C} of C12, {H12D,
H12E,H12F} of C12X, {H13A,H13B,H13C} of C13, {H14A,H14B,H14C} of C14, {H14D,
H14E,H14F} of C14X, {H23A,H23B,H23C} of C23, {H23D,H23E,H23F} of C23X, {H24A,
H24B,H24C} of C24, {H24D,H24E,H24F} of C24X
2. Restrained distances
Si3X-O8 = Si3-O8
1.7 with sigma of 0.02
Si3X-C22X = Si3-C22
1.85 with sigma of 0.01
C21-C20 = C21X-C20 = C21X-C22X = C21-C22
1.52 with sigma of 0.01
C16X-C17 = C16-C17 = C15-C16 = C15X-C16X
1.52 with sigma of 0.01
Si3-C24 = Si3X-C24X = Si3X-C23X = Si3-C23
1.54 with sigma of 0.01
Si3X-O8
with sigma of 0.001
Si3-O8 ~ Si3X_$1-O8
with sigma of 0.001
C21-C20 ~ C21X-C20 ~ C21X-C22X ~ C21-C22
with sigma of 0.001
Si3X-C22X ~ Si3-C22
with sigma of 0.001
C16-C17 ~ C16X-C17 ~ C15X-C16X ~ C15-C16
with sigma of 0.001
Si1-C11 ~ Si1-C12X ~ Si1-C12 ~ Si2-C13 ~ Si2-C14X
with sigma of 0.001
Si3-C24 ~ Si3-C23 ~ Si3X-C24X ~ Si3X-C23X
with sigma of 0.001
Si2-C15X_$2 ~ Si2-C15_$2
with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(Si3X) ~ Ueq, Uanis(Si3) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C21X) = Uiso(C21) = Uiso(C22) = Uiso(C22X)
Uanis(Si3) = Uanis(Si3X)
Uiso(C15X) = Uiso(C15) = Uiso(C16) = Uiso(C16X)
Uiso(C14) = Uiso(C14X)
Uiso(C12X) = Uiso(C12)
Uiso(C24X) = Uiso(C24) = Uiso(C23) = Uiso(C23X)
4. Others
Fixed Sof: Si3X(0.5) Si3(0.5) O8(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
C12X(0.5) H12D(0.5) H12E(0.5) H12F(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
C14X(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15(0.5) H15A(0.5) H15B(0.5) C15X(0.5)
H15C(0.5) H15D(0.5) C16(0.5) H16A(0.5) H16B(0.5) C16X(0.5) H16C(0.5) H16D(0.5)
H17C(0.5) H17D(0.5) H17A(0.5) H17B(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
H20D(0.5) C21(0.5) H21A(0.5) H21B(0.5) C21X(0.5) H21C(0.5) H21D(0.5) C22(0.5)
H22A(0.5) H22B(0.5) C22X(0.5) H22C(0.5) H22D(0.5) C23(0.5) H23A(0.5) H23B(0.5)
H23C(0.5) C23X(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C24(0.5) H24A(0.5) H24B(0.5)
H24C(0.5) C24X(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
5.a Riding coordinates:
O7(H7), N4(H4), C12(H12A,H12B,H12C), C12X(H12D,H12E,H12F), C13(H13A,H13B,
H13C), C14(H14A,H14B,H14C), C14X(H14D,H14E,H14F), C23(H23A,H23B,H23C),
C23X(H23D,H23E,H23F), C24(H24A,H24B,H24C), C24X(H24D,H24E,H24F)
5.b Secondary CH2 refined with riding coordinates:
C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C15(H15A,H15B), C15X(H15C,H15D),
C16(H16A,H16B), C16X(H16C,H16D), C17(H17C,H17D), C17(H17A,H17B), C20(H20A,
H20B), C20(H20C,H20D), C21(H21A,H21B), C21X(H21C,H21D), C22(H22A,H22B),
C22X(H22C,H22D)
5.c Aromatic/amide H refined with riding coordinates:
N2(H2), C1(H1), C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6)
5.d Idealised Me refined as rotating group:
C11(H11A,H11B,H11C)
;