Crystal structure of <i>cis</i>-[dichlorido(1,4,8,11-tetraazacyclotetradecane-<i>{κ</i>N}^4^)chromium(III)][oxalato(1,4,8,11-tetraazacyclotetradecane-<i>{κ</i>N}^4^)chromium(III)] diperchlorate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 72 (2016) 1417–1420; doi:10.1107/S2056989016014134

data_2241846
_publ_section_title
;
 Crystal structure of
 <i>cis</i>-[dichlorido(1,4,8,11-tetraazacyclotetradecane-<i>{\k</i>N}^4^)chromium(III)][oxalato(1,4,8,11-tetraazacyclotetradecane-<i>{\k</i>N}^4^)chromium(III)]
 diperchlorate from synchrotron data
;
_journal_coeditor_code           WM5323
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1417
_journal_page_last               1420
_journal_paper_doi               10.1107/S2056989016014134
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety
'[Cr Cl2 (C10 H24 N4)] [Cr(C2 O4)2 (C10 H24 N4)](Cl O4)2'
_chemical_formula_sum            'C22 H48 Cl4 Cr2 N8 O12'
_chemical_formula_weight         862.48
_chemical_name_systematic
<i>cis</i>-[dichlorido(1,4,8,11-tetraazacyclotetradecane-<i>\kN</i>^4^)chromium(III)][oxalato(1,4,8,11-tetraazacyclotetradecane-<i>\kN</i>^4^)chromium(III)]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            8
_cell_length_a                   18.599(4)
_cell_length_b                   26.986(5)
_cell_length_c                   14.042(3)
_cell_measurement_reflns_used    25281
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      33.311
_cell_measurement_theta_min      0.384
_cell_volume                     7048(3)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i> (Shin <i>et al.</i>,  2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.670
_diffrn_reflns_av_R_equivalents  0.1182
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14619
_diffrn_reflns_theta_full        23.703
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.855
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       needle
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.506
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1586 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013).
;
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4764
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0928P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                4011
_reflns_number_total             4764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5323sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        7048(2)
_cod_database_code               2241846
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.996
_shelx_hkl_checksum              3148
_shelx_res_checksum              65724
_cod_database_fobs_code 2241846