One-pot synthesis, characterisation and kinetic stability of novel side-bridged pentaazamacrocyclic copper(ii) complexes
Betts, Helen M.; Pascu, Sofia I.; Buchard, Antoine; Bonnitcha, Paul D.; Dilworth, Jonathan R.; RSC Advances 4 (2014) 12964–; doi:10.1039/c3ra47450j

data_7239473
_publ_section_title
;
 One-pot synthesis, characterisation and kinetic stability of novel
 side-bridged pentaazamacrocyclic copper(ii) complexes
;
_journal_issue                   25
_journal_name_full               'RSC Advances'
_journal_page_first              12964
_journal_paper_doi               10.1039/c3ra47450j
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C15 H29 Cl2 Cu1 N5 O4'
_chemical_formula_sum            'C15 H29 Cl2 Cu N5 O4'
_chemical_formula_weight         477.88
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-11-05
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 91.7800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9964(8)
_cell_length_b                   15.8250(11)
_cell_length_c                   21.4986(15)
_cell_measurement_reflns_used    38420
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1
_cell_volume                     4079.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6709
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38420
_diffrn_reflns_theta_full        31.532
_diffrn_reflns_theta_max         33.191
_diffrn_reflns_theta_min         3.581
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       needle
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1331
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.008182
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.08 0.952E-01 0.564 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0762
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0497
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4626
_reflns_number_total             11021
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2184(4)
_oxford_structure_analysis_title 'ox023 in P2(1)/n'
_cod_data_source_file            c3ra47450j1.txt
_cod_data_source_block           global
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C15 H29 Cl2 Cu1 N5 O4'
_cod_database_code               7239473