Structure and Magnetism of 3D Anionic Metal Dicyanamide (MePh3P)[M(dca)3] (M = Fe, Co, Ni) and (EtPh3P)[M(dca)3] (M = Mn, Co, Ni) Networks
van der Werff, Patricia M.; Batten, Stuart R.; Jensen, Paul; Moubaraki, Boujemaa; Murray, Keith S.; Cashion, John D.; Crystal Growth & Design 4 (2004) 503–; doi:10.1021/cg034258n

data_4505358
_publ_contact_author
;
    Dr. S.R. Batten
    School of Chemistry
    Monash University 3800
    AUSTRALIA
;
_publ_section_title
;
 Structure and Magnetism of 3D Anionic Metal Dicyanamide (MePh3P)[M(dca)3]
 (M = Fe, Co, Ni) and (EtPh3P)[M(dca)3] (M = Mn, Co, Ni) Networks
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              503
_journal_paper_doi               10.1021/cg034258n
_journal_volume                  4
_journal_year                    2004
_chemical_formula_sum            'C26 H20 N9 Ni P'
_chemical_formula_weight         548.19
_chemical_name_systematic
; 
 Ethyltriphenylphosphonium tris(dicyanamido)nickelate(II)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.1192(1)
_cell_length_b                   16.6545(1)
_cell_length_c                   21.5833(2)
_cell_measurement_temperature    123(2)
_cell_volume                     5075.27(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36451
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.9128
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0166P)^2^+1.6608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                9695
_reflns_number_total             11953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg034258nsi20031223_013219.cif
_cod_data_source_block           EtNi
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4505358