Solvothermal syntheses, characterizations and properties of three transition metal (Ni(ii), Co(ii)) imino-carboxylate-diphosphonates
Ma, Kuirong; Xu, Jianing; Zhang, Lirong; Shi, Jing; Zhang, Daojun; Zhu, Yulan; Fan, Yong; Song, Tianyong; New Journal of Chemistry 33 (2009) 886–; doi:10.1039/b814080d

data_7053762
_publ_section_title
;
 Solvothermal syntheses, characterizations and properties of three
 transition metal (Ni(ii), Co(ii)) imino-carboxylate-diphosphonates
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              886
_journal_paper_doi               10.1039/b814080d
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C4 H19 Co N O13 P2'
_chemical_formula_sum            'C4 H19 Co N O13 P2'
_chemical_formula_weight         410.07
_chemical_melting_point          ?
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.84(3)
_cell_angle_beta                 62.55(3)
_cell_angle_gamma                76.32(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3817(19)
_cell_length_b                   9.3988(19)
_cell_length_c                   9.776(2)
_cell_measurement_reflns_used    3405
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.99
_cell_volume                     743.1(3)
_computing_cell_refinement       Process-auto
_computing_data_collection       Process-auto
_computing_data_reduction        Process-auto
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7382
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Process-auto
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3405
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.8581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                3097
_reflns_number_total             3405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814080dsup1.cif
_cod_data_source_block           H3O[CoH2L2(H2O)2]2H2O_(3)
_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.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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 
;
_cod_original_cell_volume        743.2(3)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053762