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_7107587
_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         'C22 H30 N4 O2'
_chemical_formula_sum            'C22 H30 N4 O2'
_chemical_formula_weight         382.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-02-18
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.12 svn.r1656, GUI svn.r3487)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.910(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0103(9)
_cell_length_b                   6.5415(4)
_cell_length_c                   13.3553(9)
_cell_measurement_reflns_used    1290
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0651
_cell_measurement_theta_min      3.3442
_cell_volume                     1043.69(12)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0938
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
1 omega -7.00 23.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 18.1770 -89.0000 -38.0000 30

2 omega -91.00 5.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -18.5676 -37.0000 90.0000 96

3 omega -55.00 20.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -18.5676 89.0000 -103.0000 75
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0197016000
_diffrn_orient_matrix_UB_12      0.0940292000
_diffrn_orient_matrix_UB_13      -0.0179144000
_diffrn_orient_matrix_UB_21      -0.0175512000
_diffrn_orient_matrix_UB_22      -0.0302965000
_diffrn_orient_matrix_UB_23      -0.0501667000
_diffrn_orient_matrix_UB_31      -0.0531434000
_diffrn_orient_matrix_UB_32      0.0448204000
_diffrn_orient_matrix_UB_33      0.0038254000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4218
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             412
_exptl_crystal_recrystallization_method
'Dichloromethane and petroleum ether mixture'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0725P)^2^+0.2709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1827
_reflns_number_gt                1279
_reflns_number_total             2124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc00094f.txt
_cod_data_source_block           uni-1
_cod_database_code               7107587