Controlling the Polymorph of LnIII(NO3)3-x(OH)x[15-MCCuII(N)S-pheHA-5] Complexes through Solvent Type and LnIIIIon Choice
Zaleski, Curtis M.; Cutland-Van Noord, Annabel D.; Kampf, Jeff W.; Pecoraro, Vincent L.; Crystal Growth & Design 7 (2007) 1098–; doi:10.1021/cg060743h

data_4504063
_publ_section_title
;
 Controlling the Polymorph of LnIII(NO3)3-x(OH)x[15-MCCuII(N)S-pheHA-5]
 Complexes through Solvent Type and LnIIIIon Choice
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1098
_journal_paper_doi               10.1021/cg060743h
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety
;
           (C45H50N10O10Cu5Gd)(NO3)(H2O), (NO3), (CH3O), (H2O)9
;
_chemical_formula_sum            'C46 H73 Cu5 Gd N12 O27'
_chemical_formula_weight         1701.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_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            4
_cell_length_a                   19.2377(14)
_cell_length_b                   19.2377(14)
_cell_length_c                   18.325(3)
_cell_measurement_reflns_used    7855
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      3.17
_cell_volume                     6781.9(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      118(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84316
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  0.3057
_exptl_absorpt_correction_T_min  0.2437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       multi-faceted
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         1.061
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         16827
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+28.6801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                15911
_reflns_number_total             16827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060743hsi20061023_044727.cif
_cod_data_source_block           cz253
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_cell_volume        6781.9(12)
_cod_original_sg_symbol_H-M      P4(3)
_cod_database_code               4504063