Nickel and Cobalt Hexamethylentetramine Complexes (NO3)2Me(H2O)6(HMTA)2.4H2O (Me = Co2+, Ni2+): New Molecular Precursors for the Preparation of Metal Dispersions
Pavel Afanasiev; Sandra Chouzier; Tivadar Czeri; Guillaume Pilet; Christophe Pichon; Magalie Roy; Michel Vrinat; Inorganic Chemistry 47 (2008) 2303–2311; doi:10.1021/ic7013013

data_4304035
_publ_contact_author_address
; 
Groupe de Cristallographie et Ing\'enierie Mol\'eculaire
Laboratoire des Multimat\'eriaux et Interfaces
UMR 5615 CNRS-Universit\'e Claude Bernard Lyon 1
B\^at. Jules Raulin
43 bd du 11 Novembre 1918
69622 Villeurbanne cedex
FRANCE
;
_publ_contact_author_email       guillaume.pilet@univ-lyon1.fr
_publ_contact_author_fax         +33472431160
_publ_contact_author_name        'Guillaume Pilet'
_publ_contact_author_phone       +33472448220
_publ_section_title
;
Nickel and Cobalt Hexamethylentetramine Complexes
(NO3)2Me(H2O)6(HMTA)2.4H2O (Me = Co2+, Ni2+): New Molecular Precursors for
the Preparation of Metal Dispersions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2303
_journal_page_last               2311
_journal_paper_doi               10.1021/ic7013013
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C12 H44 Co1 N10 O16'
_chemical_formula_sum            'C12 H44 Co N10 O16'
_chemical_formula_weight         643.5
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-10-19
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                88.214(2)
_cell_angle_beta                 75.600(3)
_cell_angle_gamma                61.618(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1231(3)
_cell_length_b                   9.4137(5)
_cell_length_c                   9.6718(4)
_cell_measurement_reflns_used    2554
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1
_cell_volume                     704.13(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT. Nonius (1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4999
_diffrn_reflns_theta_full        27.020
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         2.185
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            rose
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       plate
_exptl_crystal_F_000             327.500
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.36
_refine_ls_extinction_coef       130(20)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.1214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2430
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000405
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.844 0.197 0.571 -0.124E-01 0.706E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0602
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0480
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2430
_reflns_number_total             3217
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.865(2)
_oxford_structure_analysis_title 'import in P -1'
_cod_data_source_file            ic7013013-file001.cif
_cod_data_source_block           x
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C12 H44 Co1 N10 O16'
_cod_database_code               4304035