The triclinic polymorph of dibromo[(‒)-sparteine-κ^2^<i>N</i>,<i>N</i>']zinc(II)
Alcántara-Flores, José Luis; Bernès, Sylvain; Reyes-Ortega, Yasmi; Zamorano-Ulloa, Rafael; Acta Crystallographica Section C 59 (2003) m79–m81; doi:10.1107/S0108270103001483

data_2013162
_publ_section_title
;
 The triclinic polymorph of
 dibromo[(--)-sparteine-\k^2^<i>N</i>,<i>N</i>']zinc(II)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m79
_journal_page_last               m81
_journal_paper_doi               10.1107/S0108270103001483
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Zn Br2 (C15 H26 N2)]'
_chemical_formula_moiety         'C15 H26 Br2 N2 Zn'
_chemical_formula_sum            'C15 H26 Br2 N2 Zn'
_chemical_formula_weight         459.57
_chemical_melting_point          566
_chemical_name_common            dibromo[(-)-sparteine-\k^2^N,N']zinc(II)
_chemical_name_systematic
; dibromo[(6R,7S,8S,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           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.429(6)
_cell_angle_beta                 112.808(5)
_cell_angle_gamma                110.666(6)
_cell_formula_units_Z            1
_cell_length_a                   7.4715(6)
_cell_length_b                   7.7082(7)
_cell_length_c                   9.1435(6)
_cell_measurement_reflns_used    84
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      12.96
_cell_measurement_theta_min      5.01
_cell_volume                     432.02(7)
_computing_cell_refinement       'XSCAnS 2.21 (Siemens, 1996)'
_computing_data_collection       'XSCAnS 2.21 (Siemens, 1996)'
_computing_data_reduction        'XSCAnS 2.21 (Siemens, 1996)'
_computing_molecular_graphics
' SHELXTL-Plus (Sheldrick, 1998) and Mercury 1.1 (CCDC, 2002)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4908
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.039
_exptl_absorpt_correction_T_max  0.381
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   'XSCAnS 2.21 (Siemens, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             230
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.772
_refine_ls_abs_structure_details 'Flack (1983); 2436 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.016(13)
_refine_ls_extinction_coef       0.0083(17)
_refine_ls_extinction_expression
'Fc^*^ = kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4908
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0364P)^2^+0.6283P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                4244
_reflns_number_total             4908
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1241.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               2013162
_cod_database_fobs_code          2013162