A zinc(II) directed triple-stranded helicate incorporating a nine membered metallamacrocycle: supramolecular cylinders mimicking P1 nuclease
Rakesh K. Mishra; Kaushal Kumar Upadhyay; Sachin Shukla; R. Mishra; Chem.Commun. 48 (2012) 4238–; doi:10.1039/c2cc00094f

data_7107586
_publ_section_title
;
 A zinc(II) directed triple-stranded helicate incorporating a nine
 membered metallamacrocycle: supramolecular cylinders mimicking P1
 nuclease
;
_journal_name_full               Chem.Commun.
_journal_page_first              4238
_journal_paper_doi               10.1039/c2cc00094f
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C66 H84 N12 O6 Zn3, H2 O'
_chemical_formula_sum            'C66 H86 N12 O7 Zn3'
_chemical_formula_weight         1355.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Tue Jan 18 15:56:13 2011'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.391(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0652(12)
_cell_length_b                   20.5741(9)
_cell_length_c                   19.1857(17)
_cell_measurement_reflns_used    8459
_cell_measurement_temperature    202.2
_cell_measurement_theta_max      29.2644
_cell_measurement_theta_min      2.9647
_cell_volume                     6494.4(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      202.2
_diffrn_detector_area_resol_mean 16.0938
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega 32.00 84.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 18.2130 0.0000 -120.0000 52

2 omega -12.00 14.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 18.2130 77.0000 90.0000 26

3 omega 50.00 77.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 18.2130 77.0000 90.0000 27

4 omega 8.00 79.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 18.2130 -140.0000 122.0000 71

5 omega -45.00 52.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -18.6036 77.0000 -90.0000 97
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0058310000
_diffrn_orient_matrix_UB_12      0.0305723000
_diffrn_orient_matrix_UB_13      0.0186520000
_diffrn_orient_matrix_UB_21      -0.0145835000
_diffrn_orient_matrix_UB_22      0.0158908000
_diffrn_orient_matrix_UB_23      -0.0359933000
_diffrn_orient_matrix_UB_31      -0.0401265000
_diffrn_orient_matrix_UB_32      -0.0013513000
_diffrn_orient_matrix_UB_33      -0.0022394000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.1824
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36622
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.9647
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         13252
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                8649
_reflns_number_total             13252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc00094f.txt
_cod_data_source_block           rkm-1
_cod_original_cell_volume        6494.4(8)
_cod_database_code               7107586
_chemical_oxdiff_formula         'C22 H12 O2 N2 Zn1'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32