A unique copper coordination structure with both mono- and bi-dentate ethylenediamine ligands
Sharma, Jai; Jiang, Zhelong; Bhutani, Ankita; Behera, Piush; Shoemaker, Daniel P.; CrystEngComm 21 (2019) 2718–; doi:10.1039/C8CE02188K

data_7232451
_publ_section_title
;
 A unique copper coordination structure with both mono- and bi-dentate
 ethylenediamine ligands
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2718
_journal_paper_doi               10.1039/C8CE02188K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C6 H24 Cu N6, 2(N O3)'
_chemical_formula_sum            'C6 H24 Cu N8 O6'
_chemical_formula_weight         367.87
_chemical_name_common            '[Cu(en-N)(en-N,N')](NO3)2'
_chemical_name_systematic
'(ethylenediamine-N)-bis(ethylenediamine-N,N')-copper(II) bis(nitrate)'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-16 deposited with the CCDC.    2019-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8262(5)
_cell_length_b                   9.7712(4)
_cell_length_c                   11.9065(5)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    99.96
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.62
_cell_volume                     1486.93(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  Mo_duo
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35107
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.317
_diffrn_reflns_theta_min         2.624
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1655 before and 0.0497 after correction. The Ratio of minimum to maximum transmission is 0.8190. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       needle
_exptl_crystal_F_000             772
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol, ethylenediamine'
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.093
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6107
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0178(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+0.9614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             3700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce02188k2.cif
_cod_data_source_block           dd90ls
_cod_depositor_comments          'Adding full bibliography for 7232451.cif.'
_cod_database_code               7232451
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.644
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1c,H1d), C2(H2c,H2d), C3(H3c,H3d), C4(H4c,H4d), C5(H5c,H5d), C6(H6c,H6d)
;
_olex2_submission_original_sample_id dd90L
_olex2_submission_special_instructions 'No special instructions were received'