Crystal structure of 1-{3-(11,19-dimethyl-3,7,15-triazatricyclo[15.3.1.115,13]-tetracosa-1(21),9(22),10,12,17,20-hexaene-21,22-diol)propyl}-11,19-dimethyl-3,7,15-triazatricyclo[15.3.1.115,13]-tetracosa-1(21),9(22),10,12,17,20-hexaene-21,22-dioldinickel(II) oxalate pentahydrate, Ni2(C45H62N6O4)(C2O4) · 5H2O
Huan-Huan Chen; Jin Yang; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 603–; doi:

data_8102746
_publ_section_title
;
 Crystal structure of
 1-{3-(11,19-dimethyl-3,7,15-triazatricyclo[15.3.1.115,13]-tetracosa-1(21),9(22),10,12,17,20-hexaene-21,22-diol)propyl}-11,19-dimethyl-3,7,15-triazatricyclo[15.3.1.115,13]-tetracosa-1(21),9(22),10,12,17,20-hexaene-21,22-dioldinickel(II)
 oxalate pentahydrate, Ni2(C45H62N6O4)(C2O4) &#x00B7; 5H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              603
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety
; 
C47 H62 N6 Ni2 O8, 
3.5(H2 O), 0.5(O2), 0.5(O)
;
_chemical_formula_sum            'C47 H69 N6 Ni2 O13'
_chemical_formula_weight         1043.50
_chemical_melting_point          ?
_chemical_name_common
;           
1-{3-(11,19-dimethyl-3,7,15,-triazatricyclo-[15.3.1.115,13]
tetracosa-1(21),-9(22),10,12,17,20-hexaene-
21,22-diol) propyl }-11,19-dimethyl
-3,7,15,-triazatricyclo-[15.3.1.115,13] 
tetracosa-1(21),-9(22),10,12,17,20-hexaene
-21,22-diol dinickel(II) oxalate hydrate
;
_chemical_name_systematic
;
1-{3-(11,19-dimethyl-3,7,15,-triazatricyclo-[15.3.1.115,13]
tetracosa-1(21),-9(22),10,12,17,20-hexaene-
21,22-diol) propyl }-11,19-dimethyl
-3,7,15,-triazatricyclo-[15.3.1.115,13] 
tetracosa-1(21),-9(22),10,12,17,20-hexaene
-21,22-diol dinickel(II) oxalate hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.000(5)
_cell_length_b                   12.000(5)
_cell_length_c                   24.000(5)
_cell_measurement_reflns_used    11420
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      3.1
_cell_volume                     4608(3)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46619
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.880
_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    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11420
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+2.3431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1657
_reflns_number_gt                7099
_reflns_number_total             11420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3035.cff
_cod_data_source_block           mm
_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.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

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_H-M      P2(1)/n
_cod_database_code               8102746