Crystal structures and investigation of the third-order nonlinear optical properties of four coordination polymers by using the Z-scan technique
Lian, Zhaoxun; Zhao, Ning; Liu, Ping; An, Caixia; Wang, Airong; Yang, Fengxia; CrystEngComm 20 (2018) 5833–; doi:10.1039/C8CE01283K

data_7231503
_publ_section_title
;
 Crystal structures and investigation of the third-order nonlinear optical
 properties of four coordination polymers by using the Z-scan technique
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5833
_journal_paper_doi               10.1039/C8CE01283K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C23 H20 N4 Ni O7, 2(H2 O)'
_chemical_formula_sum            'C23 H24 N4 Ni O9'
_chemical_formula_weight         559.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-02-11 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.604(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.542(13)
_cell_length_b                   10.509(6)
_cell_length_c                   10.273(6)
_cell_measurement_reflns_used    3491
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      2.36
_cell_volume                     2459(2)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_data_reduction        'XCAD (P.McArdle, 2000)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5327
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         2969
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0723P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                2644
_reflns_number_total             2969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01283k2.cif
_cod_data_source_block           07
_cod_depositor_comments
'Adding full bibliography for 7231500--7231503.cif.'
_cod_original_cell_volume        2460(2)
_cod_database_code               7231503
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.88(3) 0.12(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H8A,H8B} of O8, {H7A,H7B} of O7, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H9A,H9B} of O9
3.a Riding coordinates:
 O7(H7A,H7B), O8(H8A,H8B)
3.b Free rotating group:
 O9(H9A,H9B)
3.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4A), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              88711
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'