Hydrogen-Bonded Supramolecular Architectures Based on Tris(Hydranilato)Metallate(III) (M = Fe, Cr) Metallotectons
Atzori, Matteo; Marchiò, Luciano; Clérac, Rodolphe; Serpe, Angela; Deplano, Paola; Avarvari, Narcis; Mercuri, Maria Laura; Crystal Growth & Design 14 (2014) 5938–; doi:10.1021/cg501143z

data_4512004
_publ_section_title
;
 Hydrogen-Bonded Supramolecular Architectures Based on
 Tris(Hydranilato)Metallate(III) (M = Fe, Cr) Metallotectons
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5938
_journal_paper_doi               10.1021/cg501143z
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C90 H78 Fe O18 P3'
_chemical_formula_sum            'C90 H78 Fe O18 P3'
_chemical_formula_weight         1596.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.007(4)
_cell_angle_beta                 84.696(5)
_cell_angle_gamma                64.123(4)
_cell_formula_units_Z            2
_cell_length_a                   13.704(3)
_cell_length_b                   17.106(4)
_cell_length_c                   19.923(5)
_cell_measurement_reflns_used    16666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.728
_cell_measurement_theta_min      1.352
_cell_volume                     4094.4(17)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Breeze CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.1125
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.728
_diffrn_reflns_theta_min         1.352
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector
scaling and absorption correction. 
Before parameter refinement wR2(int) was 0.1109, and
after parameter refinement  wr2(int) was 0.0560 

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             1666
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         15587
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7158
_reflns_number_total             15587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501143z_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 4512004.cif.'
_cod_database_code               4512004