Bis(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)(μ-<small>L</small>-malato-κ^4^<i>O</i>^1^,<i>O</i>^2^:<i>O</i>^4^,<i>O</i>^4'^)dinickel(II) bis(perchlorate) monohydrate
Ou, Guang-Chuan; Zhou, Qiang; Ng, Seik Weng; Acta Crystallographica Section E 65 (2009) m728–; doi:10.1107/S1600536809020662

data_2222506
_publ_section_title
;Bis(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)(\m-<small>L</small>-malato-\k^4^<i>O</i>^1^,<i>O</i>^2^:<i>O</i>^4^,<i>O</i>^4'^)dinickel(II)
 bis(perchlorate) monohydrate
;
_journal_coeditor_code           XU2535
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m728
_journal_paper_doi               10.1107/S1600536809020662
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Ni2 (C4 H4 O5) (C16 H36 N4)2] (Cl O4)2 , H2 O'
_chemical_formula_moiety         'C36 H76 N8 Ni2 O5, 2(Cl O4 -), H2 O'
_chemical_formula_sum            'C36 H78 Cl2 N8 Ni2 O14'
_chemical_formula_weight         1035.38
_chemical_name_systematic
;
Bis(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-
\k^4^<i>N</i>)(\m-<i>L</i>-malato-\k^4^<i>O</i>^1^,<i>O</i>^2^:
<i>O</i>^4^,<i>O</i>^4'^)dinickel(II) bis(perchlorate) monohydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.562(2)
_cell_length_b                   18.984(2)
_cell_length_c                   19.350(3)
_cell_measurement_reflns_used    1019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.8
_cell_volume                     4981.9(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42585
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.381
_refine_ls_abs_structure_details 'Flack (Flack, 1983), 4936 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10997
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+1.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                7769
_reflns_number_total             10997
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu2535.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4982.0(10)
_cod_database_code               2222506
_cod_database_fobs_code          2222506