Synthesis, crystal structure and spectroscopic properties of <i>trans</i>-dibromidobis(2,2-dimethylpropane-1,3-diamine-κ^2^<i>N,N</i>')chromium(III) perchlorate
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615006026

data_2019923
_publ_section_title
;
 Synthesis, crystal structure and spectroscopic properties of
 <i>trans</i>-dibromidobis(2,2-dimethylpropane-1,3-diamine-\k^2^<i>N,N</i>')chromium(III)
 perchlorate
;
_journal_coeditor_code           EG3179
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615006026
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cr Br2 (C5 H14 N2)2] Cl O4'
_chemical_formula_moiety         'C10 H28 N4 Br2 Cr, Cl O4'
_chemical_formula_sum            'C10 H28 Br2 Cl Cr N4 O4'
_chemical_formula_weight         515.63
_chemical_name_systematic
;
trans-dibromidobis(2,2-dimethylpropane-1,3-diamine-\k^2^2N,N')chromium(III)
perchlorate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   20.656(4)
_cell_length_b                   17.666(4)
_cell_length_c                   31.305(6)
_cell_measurement_reflns_used    352345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.547
_cell_measurement_theta_min      0.361
_cell_volume                     11423(4)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection
'PAL ADSC Quantum-210 ADX (Arvai & Nielsen, 1983)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2014)'
_computing_publication_material
'publCIF (Westrip, 2010) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            115348
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.771
_exptl_absorpt_coefficient_mu    3.597
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'(HKL3000sm SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       plate
_exptl_crystal_F_000             6216
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.420
_refine_ls_extinction_coef       0.00083(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2014/7 (Sheldrick, 2015)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         15666
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0577P)^2^+5.7020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                13691
_reflns_number_total             15666
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3179sup1.cf
_cod_data_source_block           I
_cod_database_code               2019923
_cod_database_fobs_code          2019923
_shelx_estimated_absorpt_t_min   0.670
_shelx_estimated_absorpt_t_max   0.841
_shelx_hkl_checksum              28596
_shelx_res_checksum              76701