Bis(dihydrogen phosphato-<i>O</i>)[(1<i>SR</i>,4<i>SR</i>,8<i>RS</i>,11<i>RS</i>)-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>]nickel(II)
Namouchi Cherni, Saoussen; Driss, Ahmed; El Maaoui, Mohamed; Jouini, Tahar; Acta Crystallographica Section C 54 (1998) 1768–1770; doi:10.1107/S0108270198008245

data_2007909
_publ_section_title
;Bis(dihydrogen
 phosphato-<i>O</i>)[(1<i>SR</i>,4<i>SR</i>,8<i>RS</i>,11<i>RS</i>)-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>]nickel(II)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1768
_journal_page_last               1770
_journal_paper_doi               10.1107/S0108270198008245
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Ni(H2 P O4)2 (C10 H24 N4)]'
_chemical_formula_moiety         'C10 H28 N4 Ni O8 P2'
_chemical_formula_structural     '[Ni(C10H24N4)(H2PO4)2]'
_chemical_formula_sum            'C10 H28 N4 Ni O8 P2'
_chemical_formula_weight         453.01
_chemical_name_systematic
;
Bis(dihydroxophosphato)
[(1SR,4SR,8RS,11RS)-1,4,8,11-tetraazacyclotetradecane-\k^4^N]nickel(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                89.607(7)
_cell_angle_beta                 90.489(8)
_cell_angle_gamma                93.555(8)
_cell_formula_units_Z            2
_cell_length_a                   9.4915(10)
_cell_length_b                   10.3342(8)
_cell_length_c                   9.1930(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.04
_cell_measurement_theta_min      11.66
_cell_volume                     899.93(15)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection
;
CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992; Enraf-Nonius,
1994)
;
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0076
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3760
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   'empirical \y scan (North et al., 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.282
_refine_ls_extinction_coef       0.0081(8)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         3529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_obs          0.0218
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.4246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0570
_refine_ls_wR_factor_obs         0.0542
_reflns_number_observed          3127
_reflns_number_total             3529
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            da1017.cif
_cod_data_source_block           cher4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.0262P)^2^+0.4246P] 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^)+(0.0262P)^2^+0.4246P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2007909