Copper(ii) complexes of N-propargyl cyclam ligands reveal a range of coordination modes and colours, and unexpected reactivity.
Counsell, Andrew J.; Yu, Mingfeng; Shi, Mengying; Jones, Angus T.; Batten, James M.; Turner, Peter; Todd, Matthew H.; Rutledge, Peter J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3931–3942; doi:10.1039/d0dt03736b

data_7706594
_publ_section_title
;
 Copper(ii) complexes of N-propargyl cyclam ligands reveal a range of
 coordination modes and colours, and unexpected reactivity.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3931
_journal_page_last               3942
_journal_paper_doi               10.1039/d0dt03736b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C13.25 H27 Cl2 Cu N4 O8.25'
_chemical_formula_weight         508.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-28 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.422(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.689(5)
_cell_length_b                   8.5129(12)
_cell_length_c                   16.517(2)
_cell_measurement_reflns_used    7362
_cell_measurement_temperature    150.0(5)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.49
_cell_volume                     4118.9(10)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
  OLEX2 (Dolomanov,O.V.et al., 2009)
  shelXle (H\"ubschle,C.B., et al., 2011) 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'Charge Flipping (Oszl\'anyi & S\"uti\>o, 2008)'
_diffrn_ambient_temperature      150.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19982
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.895
_diffrn_reflns_theta_min         2.492
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 SADABS (Bruker,2008) was used to apply a Gaussian absorption correction
 using indexed crystal faces, followed by a multiscan absorption correction.
 A Lambda/2 correction factor = 0.0015 was applied to the data.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       plate
_exptl_crystal_F_000             2108
_exptl_crystal_preparation
;
 Attached with Exxon Paratone N oil to a short length of fibre 
 supported on a thin piece of copper wire inserted in a copper 
 mounting pin. The crystal was quenched in a cold nitrogen gas 
 stream from an Oxford Cryosystems Cryostream.
;
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.362
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5064
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0358
_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^)+(0.03P)^2^+4.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4234
_reflns_number_total             5064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03736b3.cif
_cod_data_source_block           mht10rm3m_face
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7706593--7706595.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7706594
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              76696