Novel primary amide-based cationic metal complexes: green synthesis, crystal structures, Hirshfeld surface analysis and solvent-free cyanosilylation reaction.
Markad, Datta; Khullar, Sadhika; Mandal, Sanjay K.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3743–3757; doi:10.1039/c8dt04773a

data_7049007
_publ_section_title
;
 Novel primary amide-based cationic metal complexes: green synthesis,
 crystal structures, Hirshfeld surface analysis and solvent-free
 cyanosilylation reaction.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3743
_journal_page_last               3757
_journal_paper_doi               10.1039/c8dt04773a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H24 Cu N6 O2, 2(Cl O4), 0.5(H2 O)'
_chemical_formula_sum            'C18 H25 Cl2 Cu N6 O10.5'
_chemical_formula_weight         627.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                104.90(2)
_cell_angle_beta                 100.698(19)
_cell_angle_gamma                93.163(19)
_cell_formula_units_Z            2
_cell_length_a                   10.449(9)
_cell_length_b                   10.657(10)
_cell_length_c                   12.324(11)
_cell_measurement_reflns_used    8752
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.063
_cell_measurement_theta_min      2.262
_cell_volume                     1295(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20718
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.995
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker,2014/5)'
_exptl_crystal_colour            'clear blue'
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.016
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4554
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0555P)^2^+1.1832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4094
_reflns_number_total             4554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04773a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7049003--7049007.cif.'
_cod_original_formula_sum        'C18 H25 Cl2 Cu N6 O10.50'
_cod_database_code               7049007
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 H7c-O7 \\sim O7-H7d
 with sigma of 0.001
3. Others
 Fixed Sof: O7(0.5) H7c(0.5) H7d(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C7(H7a,H7b), C8(H8a,H8b), C12(H12a,H12b), C13(H13a,H13b),
 C15(H15a,H15b)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18)
4.c X=CH2 refined with riding coordinates:
 N5(H5a,H5b), N6(H6a,H6b)
;
_shelx_res_checksum              79989
_olex2_submission_special_instructions 'No special instructions were received'