Synthesis, solution studies and structural characterisation of complexes of a mixed oxa‒aza macrocycle bearing pendant amino arms
Tei, Lorenzo; Blake, Alexander J.; Bencini, Andrea; Valtancoli, Barbara; Wilson, Claire; Schröder, Martin; Journal of the Chemical Society, Dalton Transactions  (2000) 4122–; doi:10.1039/b003352i

data_7009750
_publ_section_title
;
 Synthesis, solution studies and structural characterisation of
 complexes of a mixed oxa--aza macrocycle bearing pendant amino arms
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4122
_journal_paper_doi               10.1039/b003352i
_journal_year                    2000
_chemical_formula_sum            'C16 H38 Cl2 Cu N6 O10'
_chemical_formula_weight         608.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'CH constrained, NH from difference map'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'from difference map'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.116(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2446(13)
_cell_length_b                   13.129(2)
_cell_length_c                   20.653(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      10
_cell_volume                     2459.7(6)
_computing_cell_refinement       'STADI4 v1.07'
_computing_data_collection       'STADI4 v1.07 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED v1.09 (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL v5.03 (Sheldrick,1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Stoe Stadi-4 four circle'
_diffrn_measurement_method       omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6015
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        'linear isotropic decay 5.8'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'vibrant blue'
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    'CH riding, NH distance restraints'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4313
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+5.4953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                3568
_reflns_number_total             4313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003352i.txt
_cod_data_source_block           n3o2cu
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_torsion_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (18 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+5.4953P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+5.4953P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009750