The Ni^II^, Hg^II^ and Cu^II^ complexes of 12-membered-ring mixed-donor macrocycles
Marcus, Sebastian T.; Gahan, Lawrence R.; Bernhardt, Paul V.; Acta Crystallographica Section C 56 (2000) 655–658; doi:10.1107/S0108270100003942

data_2010998
_publ_section_title
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 The Ni^II^, Hg^II^ and Cu^II^ complexes of 12-membered-ring
 mixed-donor macrocycles
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              655
_journal_page_last               658
_journal_paper_doi               10.1107/S0108270100003942
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Cu(NO3 )(C8 H19 N3 O)(H2 O)](NO3 )'
_chemical_formula_moiety         'C8 H21 CuN4 O5 + , NO3 - '
_chemical_formula_sum            'C8 H21 Cu N5 O8'
_chemical_formula_weight         378.84
_chemical_name_systematic
;
aqua(1,7-dioxa-4-thia-10-azacyclododecane)nitratocopper(II) nitrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.627(8)
_cell_angle_beta                 112.107(9)
_cell_angle_gamma                99.509(9)
_cell_formula_units_Z            2
_cell_length_a                   8.6167(9)
_cell_length_b                   9.3975(8)
_cell_length_c                   10.1180(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     737.05(14)
_computing_cell_refinement       'SET4 in CAD4 Manual  (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD4 Manual (Enraf-Nonius, 1988)'
_computing_data_reduction        'XTAL3.2 (Hall et al., 1992)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0248
_diffrn_reflns_av_sigmaI/netI    .0157
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2774
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        <5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  .632
_exptl_absorpt_correction_T_min  .401
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             394
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .60
_exptl_crystal_size_min          .30
_refine_diff_density_max         .355
_refine_diff_density_min         -.265
_refine_ls_extinction_coef       .096(3)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          .0275
_refine_ls_R_factor_gt           .0243
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.4836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0677
_reflns_number_gt                2392
_reflns_number_total             2586
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1589.cif
_cod_data_source_block           III
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.4836P] 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^)+(0.0343P)^2^+0.4836P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        737.05(12)
_cod_database_code               2010998
_cod_database_fobs_code          2010998