Acid-induced formation of hydrogen-bonded double helix based on chiral polyphenyl-bridged bis(2,2′-bipyridine) ligands
Sham, Kiu-Chor; Yee, Chi-Chung; Pan, Yi; Lau, Kai-Chung; Yiu, Shek-Man; Kwong, Hoi-Lun; RSC Adv. 4 (2014) 14513–; doi:10.1039/C4RA00849A

data_7235515
_publ_section_title
;
 Acid-induced formation of hydrogen-bonded double helix based on chiral
 polyphenyl-bridged bis(2,2&#x2032;-bipyridine) ligands
;
_journal_issue                   28
_journal_name_full               'RSC Adv.'
_journal_page_first              14513
_journal_paper_doi               10.1039/C4RA00849A
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '2(Cl4 Fe), 2(C46 H43 N4), C4 H10 O'
_chemical_formula_sum            'C96 H96 Cl8 Fe2 N8 O'
_chemical_formula_weight         1773.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-20
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.943(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.7135(9)
_cell_length_b                   21.8661(6)
_cell_length_c                   15.6061(5)
_cell_measurement_reflns_used    12497
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5678
_cell_measurement_theta_min      3.5957
_cell_volume                     10290.2(5)
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   33.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -180.0000 30

  2 omega  -24.00   33.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -60.0000 57

  3 omega   34.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 29

  4 omega   32.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 27

  5 omega -101.00  -18.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000  -60.0000 83

  6 omega -129.00  -78.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000   30.0000 51

  7 omega -128.00    5.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -12.0000  150.0000 133

  8 omega   41.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   90.0000 30

  9 omega   40.00   65.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -30.0000 25

 10 omega   42.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 28

 11 omega   44.00  146.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -180.0000 102

 12 omega   88.00  147.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000  120.0000 59

 13 omega   38.00   64.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 26

 14 omega   37.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 29

 15 omega   45.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -30.0000 25

 16 omega   38.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  150.0000 28

 17 omega   45.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 25

 18 omega   39.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 32

 19 omega   39.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 32

 20 omega   85.00  172.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   30.0000 87

 21 omega   38.00   65.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -120.0000 27

 22 omega   52.00  100.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000 -180.0000 48

 23 omega  -21.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 90

 24 omega  -69.00   21.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 90

 25 omega -125.00  -83.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -77.0000  -30.0000 42
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0416790000
_diffrn_orient_matrix_UB_12      -0.0378172000
_diffrn_orient_matrix_UB_13      -0.0055200000
_diffrn_orient_matrix_UB_21      -0.0211255000
_diffrn_orient_matrix_UB_22      -0.0563552000
_diffrn_orient_matrix_UB_23      0.0350905000
_diffrn_orient_matrix_UB_31      -0.0206621000
_diffrn_orient_matrix_UB_32      -0.0187648000
_diffrn_orient_matrix_UB_33      -0.0941028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24178
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.60
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    4.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23191
_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            yellow
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         14245
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0514
_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^)+(0.1023P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                12419
_reflns_number_total             14245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra00849a2.cif
_cod_data_source_block           061112a_jeff
_cod_database_code               7235515
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13