New Zn(II) Coordination Polymers Constructed from Amino-Alcohols and Aromatic Dicarboxylic Acids: Synthesis, Structure, Photocatalytic Properties, and Solid-State Conversion to ZnO
Paraschiv, Carmen; Cucos, Andrei; Shova, Sergiu; Madalan, Augustin M.; Maxim, Catalin; Visinescu, Diana; Cojocaru, Bogdan; Parvulescu, Vasile I.; Andruh, Marius; Crystal Growth & Design 15 (2015) 799–; doi:10.1021/cg501604c

data_4512566
_publ_section_title
;
 New Zn(II) Coordination Polymers Constructed from Amino-Alcohols and
 Aromatic Dicarboxylic Acids: Synthesis, Structure, Photocatalytic
 Properties, and Solid-State Conversion to ZnO
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              799
_journal_paper_doi               10.1021/cg501604c
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C36 H40 N2 O19 Zn5, 2.6(H2 O)'
_chemical_formula_sum            'C36 H45.2 N2 O21.6 Zn5'
_chemical_formula_weight         1178.39
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                76.057(11)
_cell_angle_beta                 86.390(11)
_cell_angle_gamma                67.910(12)
_cell_formula_units_Z            2
_cell_length_a                   13.6546(18)
_cell_length_b                   14.2126(18)
_cell_length_c                   14.6377(19)
_cell_measurement_reflns_used    2307
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      25.3130
_cell_measurement_theta_min      1.7830
_cell_volume                     2553.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.05(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -24.00   21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352  -99.0000  -90.0000 45

  2 omega   -7.00   23.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352  -99.0000    0.0000 30

  3 omega  -72.00  -37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352 -178.0000 -150.0000 35

  4 omega    0.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570   38.0000 -180.0000 85

  5 omega  -41.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570  -57.0000    0.0000 66

  6 omega  -22.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570  -99.0000 -120.0000 73

  7 omega   -4.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570  -19.0000    0.0000 43
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0271212000
_diffrn_orient_matrix_UB_12      0.0172834000
_diffrn_orient_matrix_UB_13      0.0281102000
_diffrn_orient_matrix_UB_21      -0.0291944000
_diffrn_orient_matrix_UB_22      0.0525959000
_diffrn_orient_matrix_UB_23      -0.0231048000
_diffrn_orient_matrix_UB_31      -0.0394704000
_diffrn_orient_matrix_UB_32      0.0023098000
_diffrn_orient_matrix_UB_33      0.0342222000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1686
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12760
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         12782
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                7884
_reflns_number_total             12782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501604c_si_003.cif
_cod_data_source_block           shi_2295_maan_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 4512564--4512566.cif.'
_cod_original_formula_sum        'C36 H45.20 N2 O21.60 Zn5'
_cod_database_code               4512566
_chemical_oxdiff_formula         'C25 H30 N2 O8 Zn'
_chemical_oxdiff_usercomment     TIFT
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H9WA-H9WB
 1.45 with sigma of 0.01
 O9W-H9WB = O9W-H9WA
 0.86 with sigma of 0.01
 O7W-H7WB = O7W-H7WA
 0.86 with sigma of 0.01
 H7WA-H7WB
 1.45 with sigma of 0.01
 O8W-H8WA = O8W-H8WB
 0.86 with sigma of 0.01
 H8WA-H8WB
 1.45 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 O18-H18
 0.85 with sigma of 0.01
 C18-H8
 1.919011 with sigma of 0.02
 Zn3-H8
 2.769068 with sigma of 0.02
 C35-H18
 1.887559 with sigma of 0.02
 Zn1-H18
 2.802417 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C15) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O9) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C29)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O14W(0.15) H14A(0.15) H14B(0.15) O10W(0.25) H10A(0.25) H10B(0.25)
 O4W(0.25) H4WA(0.25) H4WB(0.25) O2W(0.25) H2WA(0.25) H2WB(0.25) O11W(0.15)
 H11A(0.15) H11B(0.15) O6W(0.25) H6WA(0.25) H6WB(0.25) O9W(0.25) H9WA(0.25)
 H9WB(0.25) O12W(0.15) H12A(0.15) H12B(0.15) O7W(0.15) H7WA(0.15) H7WB(0.15)
 O8W(0.1) H8WA(0.1) H8WB(0.1) O13W(0.25) H13A(0.25) H13B(0.25) O5W(0.25)
 H5WA(0.25) H5WB(0.25) O3W(0.15) H3WA(0.15) H3WB(0.15)
5.a Riding coordinates:
 O14W(H14A,H14B), O10W(H10A,H10B), O4W(H4WA,H4WB), O2W(H2WA,H2WB), O11W(H11A,
 H11B), O6W(H6WA,H6WB), O9W(H9WA,H9WB), O12W(H12A,H12B), O7W(H7WA,H7WB),
 O8W(H8WA,H8WB), O13W(H13A,H13B), O5W(H5WA,H5WB), O3W(H3WA,H3WB)
5.b Rotating group:
 O1W(H1WA,H1WB)
5.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C21(H21A,H21B), C32(H32A,H32B), C18(H18A,H18B), C34(H34A,
 H34B), C16(H16A,H16B), C17(H17A,H17B), C20(H20A,H20B), C19(H19A,H19B),
 C35(H35A,H35B), C36(H36A,H36B), C33(H33A,H33B)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C25(H25), C5(H5), C28(H28), C29(H29), C3(H3), C12(H12),
 C4(H4), C27(H27), C14(H14), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'