Dichloro[(6<i>R</i>,7<i>S</i>,8<i>S</i>,14<i>R</i>)-({-})-α-isosparteine-κ^2^<i>N,N</i>']zinc(II)
Alcántara-Flores, José Luis; Bernès, Sylvain; Reyes-Ortega, Yasmi; Zamorano-Ulloa, Rafael; Acta Crystallographica Section E 59 (2003) m988–m990; doi:10.1107/S1600536803022414

data_2202440
_publ_section_title
Dichloro[(6<i>R</i>,7<i>S</i>,8<i>S</i>,14<i>R</i>)-({-})-\a-isosparteine-\k^2^<i>N,N</i>']zinc(II)
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m988
_journal_page_last               m990
_journal_paper_doi               10.1107/S1600536803022414
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Zn Cl2 (C15 H26 N2)]'
_chemical_formula_moiety         'C15 H26 Cl2 N2 Zn'
_chemical_formula_sum            'C15 H26 Cl2 N2 Zn'
_chemical_formula_weight         370.65
_chemical_melting_point_gt       673
_chemical_name_common
' dichloro[(6R,7S,8S,14R)-(-)-\a-isosparteine-\k^2^N,N']zinc(II)'
_chemical_name_systematic
; dichloro[(6R,7S,8R,14S)-1,3,4,7,7a,8,9,10,11,13,14,14a-dodecahydro-7,14-
methano-2H,6H-dipyrido[1,2-a;1',2'-e][1,5]diazocine-\k^2^N,N']zinc(II)
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0474(7)
_cell_length_b                   8.0474(7)
_cell_length_c                   25.518(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      12.35
_cell_measurement_theta_min      3.91
_cell_volume                     1652.6(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            6151
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.195
_refine_ls_abs_structure_details 'Flack (1983), 535 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL-Plus
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0202P)^2^+0.647P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                1184
_reflns_number_total             1467
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6282.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '> 673' was changed to
'673' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '> 673' was changed to
'673' - it should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Tetragonal' changed to
'tetragonal' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P43 21 2'
_cod_database_code               2202440
_cod_database_fobs_code          2202440