Crystallisation of H3BTC, H3TPO or H2SDA with MII (M = Co, Mn or Zn) and 2,2′-bipyridyl: design and control of co-ordination architecture, and magnetic properties (H3BTC = benzene-1,3,5-tricarboxylic acid, H3TPO = tris(4-carboxylphenyl)phosphine oxide, H2SDA = cis-stilbene-4,4′-dicarboxylic acid) †
Plater, M. John; Foreman, Mark R. St. J.; Coronado, Eugenio; Gómez-García, Carlos J.; Slawin, Alexandra M. Z.; Journal of the Chemical Society, Dalton Transactions  (1999) 4209–; doi:10.1039/a905332h

data_7027670
_publ_section_title
;
 Crystallisation of H3BTC, H3TPO or H2SDA with MII (M&#x2005;=&#x2005;Co,
 Mn or Zn) and 2,2&#x2032;-bipyridyl: design and control of co-ordination
 architecture, and magnetic properties
 (H3BTC&#x2005;=&#x2005;benzene-1,3,5-tricarboxylic acid,
 H3TPO&#x2005;=&#x2005;tris(4-carboxylphenyl)phosphine oxide,
 H2SDA&#x2005;=&#x2005;cis-stilbene-4,4&#x2032;-dicarboxylic
 acid)&#x200A;&#x2020;
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4209
_journal_paper_doi               10.1039/a905332h
_journal_year                    1999
_chemical_compound_source        -
_chemical_formula_analytical     'C62 H54 Co3 N4 O21 P2'
_chemical_formula_moiety         'C62 H54 Co3 N4 O21 P2'
_chemical_formula_structural     'C62 H54 Co3 N4 O21 P2'
_chemical_formula_sum            'C62 H54 Co3 N4 O21 P2'
_chemical_formula_weight         1429.82
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                110.791(2)
_cell_angle_beta                 93.6520(10)
_cell_angle_gamma                99.355(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9103(10)
_cell_length_b                   11.4372(11)
_cell_length_c                   13.7163(13)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      337
_cell_measurement_theta_min      23
_cell_volume                     1565.1(3)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.1239
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9933
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.764871
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            pink/orange
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       needle
_exptl_crystal_F_000             733
_exptl_crystal_size_max          .08
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.742
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0043(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7016
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_obs          0.0736
_refine_ls_shift/esd_max         -0.200
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2604
_refine_ls_wR_factor_obs         0.1997
_reflns_number_observed          3509
_reflns_number_total             7016
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905332hsup1.cif
_cod_data_source_block           11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-' 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 '-' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027670