Exploiting dimensional variability in coordination polymers: solvent promotes reversible conversion between 3D and chiral 1D architectures.
Rancan, Marzio; Armelao, Lidia; Chemical communications (Cambridge, England) 51 (2015) 12947–12949; doi:10.1039/c5cc04349b

data_7117594
_publ_section_title
;
 Exploiting dimensional variability in coordination polymers: solvent
 promotes reversible conversion between 3D and chiral 1D architectures.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12947
_journal_page_last               12949
_journal_paper_doi               10.1039/c5cc04349b
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'C46 H50 Cl Cu2 N8 O7 S3, 2(C2 H6 O S), 3(Cl O4)'
_chemical_formula_sum            'C50 H62 Cl4 Cu2 N8 O21 S5'
_chemical_formula_weight         1540.25
_chemical_name_systematic        'compound 1'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-25
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-25 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0973(2)
_cell_length_b                   28.4369(4)
_cell_length_c                   28.5016(3)
_cell_measurement_reflns_used    30275
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      27.6290
_cell_measurement_theta_min      2.3240
_cell_volume                     14667.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      301(2)
_diffrn_detector_area_resol_mean 8.0637
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
  1 omega  -54.00  105.00   0.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.1562   77.0000  -90.0000 795

  2 omega  -54.00  105.00   0.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.1562   77.0000    0.0000 795

  3 omega  -90.00   70.00   0.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -35.3649   77.0000  120.0000 800

  4 omega  -19.00  141.00   0.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       35.6774   77.0000   60.0000 800

  5 omega  -19.00  141.00   0.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       35.6774   77.0000    0.0000 800

  6 omega  -19.00  141.00   0.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       35.6774   77.0000 -180.0000 800

  7 omega  -25.00   67.00   0.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.1562  -99.0000   60.0000 460

  8 omega   -5.00   78.00   0.2000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.1562 -121.0000 -125.0000 415

  9 omega -143.00  -95.00   0.2000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -35.3649 -154.0000   76.0000 240
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0325536000
_diffrn_orient_matrix_UB_12      0.0136318000
_diffrn_orient_matrix_UB_13      -0.0026679000
_diffrn_orient_matrix_UB_21      0.0010348000
_diffrn_orient_matrix_UB_22      0.0037919000
_diffrn_orient_matrix_UB_23      0.0245843000
_diffrn_orient_matrix_UB_31      0.0217968000
_diffrn_orient_matrix_UB_32      -0.0205454000
_diffrn_orient_matrix_UB_33      0.0027853000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_laue_measured_fraction_full 0.982
_diffrn_reflns_laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            16901
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.231
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'intense violet'
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.583
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         16901
_refine_ls_number_restraints     823
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.1141
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1886P)^2^+69.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3251
_refine_ls_wR_factor_ref         0.3447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11937
_reflns_number_total             16901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04349b2.cif
_cod_data_source_block           compound_1
_cod_database_code               7117594
_reflns_odcompleteness_completeness 97.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O18-O20 = O18-O21 = O18-O19 = O20-O21 = O20-O19 = O21-O19
 2.25 with sigma of 0.01
 O4-O5 = O4-O6 = O4-O7 = O5-O6 = O5-O7 = O6-O7
 2.25 with sigma of 0.01
 O4-O5A = O4-O6A = O4-O7A = O5A-O6A = O5A-O7A = O6A-O7A
 2.25 with sigma of 0.01
 S2A-O3 \\sim S2B-O3
 with sigma of 0.02
 S3B-O1 \\sim S3B-O1
 with sigma of 0.02
 Cl2-O20 \\sim Cl2-O19 \\sim Cl2-O18 \\sim Cl2-O21
 with sigma of 0.01
 Cl1-O4 \\sim Cl1-O5 \\sim Cl1-O7A \\sim Cl1-O7 \\sim Cl1-O6A \\sim Cl1-O6
\\sim Cl1-O5A
 with sigma of 0.02
 Cl4-O10 \\sim Cl4-O11 \\sim Cl4-O12 \\sim Cl4-O13
 with sigma of 0.02
 O11-O12 \\sim O11-O10 \\sim O13-O12 \\sim O13-O12 \\sim O10-O13
 with sigma of 0.005
 S3B-C41B \\sim S3B-C40B \\sim S3A-C41A \\sim S3A-C40A
 with sigma of 0.02
 S2B-C43B \\sim S2A-C43A
 with sigma of 0.02
 S2A-C43A \\sim S2B-C43B \\sim S2B-C42 \\sim S2A-C42
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C44, Cu2, N6, N5, N8, N7, O1, O4, C14, C13, C9, C8, C12, C11, C16, C15, S3B,
 S3A, Cl1, H14, H13, H9, C10, C7, H8, H12, H11, H16, C17, C18, H15, C40B, C41B,
 C40A, C41A, O5, O7, O6, O5A, O6A, O7A, C6, H10, H7, C19, H17, H18, H40A, H40B,
 H40C, H41A, H41B, H41C, H40D, H40E, H40F, H41D, H41E, H41F, C3, C20, C4, C2,
 C23, C21, H4, C5, H2, C1, H23, C24, H21, C22, N3, H5, H1, H24, H22, Cu1, N4,
 N1, N2, O3, O2, C34, C33, C25, C29, S2B, S2A, S1, H34, C36, H33, C35, C26, H25,
  C28, H29, C42, C43B, C43A, C45, C2AA, H36, H35, C27, H26, H28, H42D, H42E,
 H42F, H42A, H42B, H42C, H43A, H43B, H43C, H43D, H43E, H43F, H45A, H45B, H45C,
 H44A, H44B, H44C, C37, C30, C39, C38, C31, C32, H39, H38, H31, H32, O17, Cl3,
 O14, O16, O15, S4, O9, C46, C47, H46A, H46B, H46C, H47A, H47B, H47C, O8, S5,
 C0BA, C7AA, H0BA, H0BB, H0BC, H7AA, H7AB, H7AC, O19, Cl2, O21, O18, O20, O10,
 Cl4, O13, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S2B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(S2A)=FVAR(1)
 Sof(S3B)=1-FVAR(2)
 Sof(S3A)=FVAR(2)
 Sof(O5A)=Sof(O6A)=Sof(O7A)=1-FVAR(3)
 Sof(O5)=Sof(O7)=Sof(O6)=FVAR(3)
 Sof(C40B)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41B)=Sof(H41A)=Sof(H41B)=
 Sof(H41C)=1-FVAR(4)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=FVAR(4)
 Sof(C43B)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(5)
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(5)
5.a Me refined with riding coordinates:
 C42(H42D,H42E,H42F), C42(H42A,H42B,H42C)
5.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C16(H16), C18(H18), C4(H4), C9(H9), C34(H34), C28(H28), C33(H33),
 C14(H14), C10(H10), C12(H12), C2(H2), C36(H36), C31(H31), C32(H32), C5(H5),
 C23(H23), C7(H7), C1(H1), C35(H35), C11(H11), C38(H38), C13(H13), C26(H26),
 C8(H8), C15(H15), C17(H17), C25(H25), C21(H21), C29(H29), C24(H24), C22(H22)
5.c Idealised Me refined as rotating group:
 C0BA(H0BA,H0BB,H0BC), C46(H46A,H46B,H46C), C7AA(H7AA,H7AB,H7AC), C40B(H40A,
 H40B,H40C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C),
 C43B(H43A,H43B,H43C), C41B(H41A,H41B,H41C), C40A(H40D,H40E,H40F), C41A(H41D,
 H41E,H41F), C43A(H43D,H43E,H43F)

SOLVENT MASK
use_set_completion: True
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
    C    Cl    Cu     H     N     O     S
 1.70  1.75  1.40  1.09  1.55  1.52  1.80

Total solvent accessible volume / cell = 1786.3 Ang^3 [12.2%]
Total electron count / cell = 392.4

Void  Vol/Ang^3  #Electrons
   1      446.6        111.7
   2      446.6        111.3
   3      446.6        112.1
   4      446.6        111.7

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