Preparation and Structure of Three Solvatomorphs of the Polymer [Co(dbm)2(4ptz)]n: Spin Canting Depending on the Supramolecular Organization
Barrios, Leoní A.; Ribas, Joan; Aromí, Guillem; Ribas-Ariño, Jordi; Gamez, Patrick; Roubeau, Olivier; Teat, Simon J.; Inorganic Chemistry 46 (2007) 7154–7162; doi:10.1021/ic7004979

data_4333279
_publ_section_title
;
 Preparation and Structure of Three Solvatomorphs of the Polymer
 [Co(dbm)2(4ptz)]n:&#x00A0; Spin Canting Depending on the Supramolecular
 Organization
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7154
_journal_page_last               7162
_journal_paper_doi               10.1021/ic7004979
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C57 H55 Co N9 O7'
_chemical_formula_weight         1037.03
_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-97
_cell_angle_alpha                94.089(2)
_cell_angle_beta                 101.607(2)
_cell_angle_gamma                112.116(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8982(11)
_cell_length_b                   14.1768(11)
_cell_length_c                   15.0948(11)
_cell_measurement_reflns_used    7634
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.31
_cell_measurement_theta_min      3.78
_cell_volume                     2663.3(4)
_computing_cell_refinement       'Bruker SAINT v7.23a'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT v7.23a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'SIR97 through WINGX'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78480
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24629
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         33.06
_diffrn_reflns_theta_min         3.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.986
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         13573
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+2.1074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                10580
_reflns_number_total             13573
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic7004979sup1.cif
_cod_data_source_block           gas4602
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333279