Crystal structure of diaqua[m-11,23-dimethyl-3,7,15,19-tetraazatricyclo[19.3.1.19,13]tetracosa-1(24),9(25),10,12,21,23-hexaene-25,26-diol]-(hydrogen 1,3,5-benzenetricarboxylato)dinickel(II) sesquihydrate, Ni2(H2O)2(C24H34N4O2)(C9H4O6) · 1.5H2O
Huan-Huan Chen; Ying-Ying Liu; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 524–; doi:

data_8102771
_publ_section_title
;
 Crystal structure of
 diaqua[m-11,23-dimethyl-3,7,15,19-tetraazatricyclo[19.3.1.19,13]tetracosa-1(24),9(25),10,12,21,23-hexaene-25,26-diol]-(hydrogen
 1,3,5-benzenetricarboxylato)dinickel(II) sesquihydrate,
 Ni2(H2O)2(C24H34N4O2)(C9H4O6) &#x00B7; 1.5H2O
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_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              524
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         '2(C33 H42 N4 Ni2 O10), 3(H2 O)'
_chemical_formula_sum            'C66 H90 N8 Ni4 O23'
_chemical_formula_weight         1598.30
_chemical_melting_point          ?
_chemical_name_common
;
[\m-11,23-dimethyl-3,7,15,19-tetraazatricyclo[19.3.1.1^9,13^]tetracosa-1(24),-
9(25),10,12,21,23-hexaene-25,26-diol]dinickel(II) hydrate --1,3,5-benzene
tricarboxylic acid -- water(1:1.5) [Ni~4~(C~24~H~34~N~4~O~2~)~2~]
(C~9~H~6~O~6~)~2~(H~2~O)~4~ ? 3H~2~O
;
_chemical_name_systematic
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[\m-11,23-dimethyl-3,7,15,19-tetraazatricyclo[19.3.1.1^9,13^]tetracosa-1(24),-
9(25),10,12,21,23-hexaene-25,26-diol]dinickel(II) hydrate --1,3,5-benzene
tricarboxylic acid -- water(1:1.5) [Ni~4~(C~24~H~34~N~4~O~2~)~2~]
(C~9~H~6~O~6~)~2~(H~2~O)~4~ ? 3H~2~O
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 101.778(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   10.531(5)
_cell_length_b                   20.032(5)
_cell_length_c                   17.057(5)
_cell_measurement_reflns_used    8015
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     3523(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33629
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Higashi,T (1995) Program for absorption correction. 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8015
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+3.2800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                5763
_reflns_number_total             8015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3068.cff
_cod_data_source_block           mm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8102771