A snapshot of a coordination polymer self-assembly process: the crystallization of a metastable 3D network followed by the spontaneous transformation in water to a 2D pseudopolymorphic phase.
Bataille, Thierry; Costantino, Ferdinando; Ienco, Andrea; Guerri, Annalisa; Marmottini, Fabio; Midollini, Stefano; Chemical communications (Cambridge, England)  (2008) 6381–6383; doi:10.1039/b813222d

data_7103590
_publ_section_title
;
 A snapshot of a coordination polymer self-assembly process: the
 crystallization of a metastable 3D network followed by the spontaneous
 transformation in water to a 2D pseudopolymorphic phase.
;
_journal_issue                   47
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6381
_journal_page_last               6383
_journal_paper_doi               10.1039/b813222d
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C96 H88 Cu4 N8 O16 P8, 14(H2 O)'
_chemical_formula_sum            'C96 H116 Cu4 N8 O30 P8'
_chemical_formula_weight         2363.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-08-04T17:27:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.196(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.8450(10)
_cell_length_b                   13.503(5)
_cell_length_c                   22.0100(10)
_cell_measurement_reflns_used    11444
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5746
_cell_measurement_theta_min      3.7266
_cell_measurement_wavelength     0.71073
_cell_volume                     5559(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.2 (release 07-07-2006 CrysAlis171 .NET)
(compiled Jul 10 2006,00:11:42)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.2 (release 07-07-2006 CrysAlis171 .NET)
(compiled Jul 10 2006,00:11:42)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.2 (release 07-07-2006 CrysAlis171 .NET)
(compiled Jul 10 2006,00:11:42)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Xcalibur3 4 circles diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0343306456
_diffrn_orient_matrix_UB_12      -0.018427972
_diffrn_orient_matrix_UB_13      -0.0219414966
_diffrn_orient_matrix_UB_21      0.0111307694
_diffrn_orient_matrix_UB_22      -0.0485368386
_diffrn_orient_matrix_UB_23      0.0125286348
_diffrn_orient_matrix_UB_31      -0.0115667969
_diffrn_orient_matrix_UB_32      0.0078311476
_diffrn_orient_matrix_UB_33      0.0253820511
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.1288
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38395
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_correction_T_min  0.9884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.2 (release 07-07-2006 CrysAlis171 .NET)
(compiled Jul 10 2006,00:11:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881 , 6030 Friedel pairs'
_refine_ls_abs_structure_Flack   0.538(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1167
_refine_ls_number_reflns         20710
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+20.3619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.2068
_reflns_number_gt                13285
_reflns_number_total             20710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813222d.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7103590