Crystal structures of two cross-bridged chromium(III) tetraazamacrocycles
Prior, Timothy J.; Maples, Danny L.; Maples, Randall D.; Hoffert, Wesley A.; Parsell, Trenton H.; Silversides, Jon D.; Archibald, Stephen J.; Hubin, Timothy J.; Acta Crystallographica Section E 70 (2014) 148–152; doi:10.1107/S1600536814019072

data_2239939
_publ_section_title
;
 Crystal structures of two cross-bridged chromium(III) tetraazamacrocycles
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              148
_journal_page_last               152
_journal_paper_doi               10.1107/S1600536814019072
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cr Cl2 (C14 H30 N4)] P F6'
_chemical_formula_moiety         'C14 H30 Cl2 Cr N4 +, F6 P -'
_chemical_formula_sum            'C14 H30 Cl2 Cr F6 N4 P'
_chemical_formula_weight         522.29
_chemical_name_systematic
'Dichlorido(4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane)chromium(III) hexafluorophosphate'
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.028(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6801(19)
_cell_length_b                   12.437(2)
_cell_length_c                   12.3864(17)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.60
_cell_volume                     2061.1(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13450
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.249
_diffrn_reflns_theta_min         2.600
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.9006
_exptl_absorpt_correction_T_min  0.7776
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[a face-indexed absorption correction was applied;
X-AREA (Stoe & Cie, 2002)]
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.786
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                2073
_reflns_number_total             4158
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5051sup1.cif
_cod_data_source_block           II
_cod_database_code               2239939
_cod_database_fobs_code          2239939
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.945
_shelx_hkl_checksum              45937
_shelx_res_checksum              72145
_shelxl_version_number           .2013