Crystal engineering of a 3-D coordination polymer from 2-D building blocks
Prior, Timothy J.; Rosseinsky, Matthew J.; Chemical Communications  (2001) 495–; doi:10.1039/b009455m

data_7114930
_publ_contact_author
;
Matthew J. Rosseinsky
Department of Chemistry 
University of Liverpool
Liverpool
L69 7ZD
UK
;
_publ_section_title
;
 Crystal engineering of a 3-D coordination polymer from 2-D building
 blocks
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              495
_journal_paper_doi               10.1039/b009455m
_journal_year                    2001
_chemical_formula_structural
'Ni 1.5 (C 9 H 3 O 6) (C 5 N 2 H 6)3.3(C 4 H 10 O)(H 2 O)'
_chemical_formula_sum            'C36 H53 N6 Ni1.5 O10'
_chemical_formula_weight         818.015
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 108.9670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1698(9)
_cell_length_b                   19.1965(12)
_cell_length_c                   16.6969(11)
_cell_measurement_reflns_used    14214
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      3.10
_cell_volume                     3992.0(5)
_computing_cell_refinement       'LSCELL (Clegg, 1997)'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics    'Diamond (Brandenburg)'
_computing_publication_material  'Stoe X-step'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.778
_diffrn_measurement_device_type  'Bruker AXS SMART CCD diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6923
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13204
_diffrn_reflns_theta_full        24.60
_diffrn_reflns_theta_max         30.24
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M., SADABS; Universitat Gottingen, 1997'
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.694
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9505
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2222
_reflns_number_gt                7586
_reflns_number_total             9505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009455m.txt
_cod_data_source_block           (Ni3(btc)2(4-AP)6.(BuOH)6(H2O)2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114930
_refine_ls_weighting_scheme_details
'w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+20.8156P] where P=(Fo^2^+2Fc^2^)/3'
_diffrn_measured_theta_max       30.24