Synthesis of Cu(II)-Organophosphonate Framework with Predefined Void Spaces
Bulut, Aysun; Zorlu, Yunus; Kirpi, Erdoğan; Çetinkaya, Ahmet; Wörle, Michael; Beckmann, Jens; Yücesan, Gündoğ; Crystal Growth & Design 15 (2015) 5665–; doi:10.1021/acs.cgd.5b01319

data_4516537
_publ_section_title
;
 Synthesis of Cu(II)-Organophosphonate Framework with Predefined Void
 Spaces
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5665
_journal_paper_doi               10.1021/acs.cgd.5b01319
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety
'C25 H22 P4 O12, C25 H21 P4 O12, 2(Cu N3 H11 O12) , 4.25(H2 O), H3 O'
_chemical_formula_sum            'C80 H76.5 Cu2 N6 O29.25 P8'
_chemical_formula_weight         1964.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.5949(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1943(9)
_cell_length_b                   23.6474(14)
_cell_length_c                   25.3309(15)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100(2)
_cell_volume                     8189.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            94667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.876
_diffrn_reflns_theta_min         1.199
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6801
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0510 before and 0.0463 after correction.
The Ratio of minimum to maximum transmission is 0.9118.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       plate
_exptl_crystal_F_000             4042
_exptl_crystal_recrystallization_method 'crystallized from water'
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         23414
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+5.5491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19415
_reflns_number_total             23414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01319_si_002.cif
_cod_data_source_block           gun12o12
_cod_original_formula_sum        'C80 H76.50 Cu2 N6 O29.25 P8'
_cod_database_code               4516537
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O3W-H3WC
 0.96142 with sigma of 0.001
 H3WA-H3WB = H3WA-H3WC = H3WB-H3WC
 1.64893 with sigma of 0.001
3. Others
 Fixed Sof: O2W(0.75) H2WA(0.75) H2WB(0.75) O2WA(0.25) H2WC(0.25) H2WD(0.25)
 H1(0.5) H2(0.5) H5(0.5) H6(0.5) O1W(0.25) H1WA(0.25) H1WB(0.25)
4.a Free rotating group:
 O6W(H6WA,H6WB), O2W(H2WA,H2WB), O2WA(H2WC,H2WD), O5W(H5WA,H5WB), O1W(H1WA,
 H1WB), O4W(H4WA,H4WB)
4.b Aromatic/amide H refined with riding coordinates:
 C3A(H3AA), C4A(H4AA), C6A(H6AB), C7A(H7AB), C9A(H9A), C10A(H10A), C12A(H12B),
 C13A(H13A), C15A(H15A), C16A(H16A), C18A(H18A), C19A(H19A), C21A(H21A),
 C22A(H22A), C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A),
 C29A(H29A), C32A(H32A), C33A(H33A), C34A(H34A), C37A(H37A), C38A(H38A),
 C39A(H39A), C40A(H40A), C3(H3A), C4(H4A), C6(H6A), C7(H7A), C9(H9), C10(H10),
 C12(H12A), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21),
 C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32),
  C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40)
4.c Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O2A(H2A), O6A(H6AA), O7A(H7AA), O11A(H11A), O1(H1), O2(H2), O3(H3),
 O4(H4), O5(H5), O6(H6), O7(H7), O12(H12)
;
_shelx_res_checksum              41379
_shelx_hkl_checksum              65420
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'