Crystalline and permanently porous porphyrin-based metal tetraphosphonates.
Rhauderwiek, Timo; Wolkersdörfer, Konrad; Øien-Ødegaard, Sigurd; Lillerud, Karl-Petter; Wark, Michael; Stock, Norbert; Chemical communications (Cambridge, England) 54 (2018) 389–392; doi:10.1039/c7cc07766a

data_7120965
_publ_section_title
;
 Crystalline and permanently porous porphyrin-based metal
 tetraphosphonates.
;
_journal_issue                   4
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              389
_journal_page_last               392
_journal_paper_doi               10.1039/c7cc07766a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C44 H24 N4 Ni2 O13 P4, O, 1.5(C)'
_chemical_formula_sum            'C45.5 H24 N4 Ni2 O14 P4'
_chemical_formula_weight         1091.95
_chemical_name_common            Ni-CAU-29
_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   mixed
_audit_creation_date             2017-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                94.723(9)
_cell_angle_beta                 97.602(9)
_cell_angle_gamma                97.880(9)
_cell_formula_units_Z            2
_cell_length_a                   9.561(5)
_cell_length_b                   15.086(9)
_cell_length_c                   16.722(9)
_cell_measurement_reflns_used    1296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.156
_cell_measurement_theta_min      2.48
_cell_volume                     2356(2)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS, 2016)'
_computing_data_reduction        'APEX3 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Diamond v4 (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 13.6986
_diffrn_detector_type            'Marmosaic 225'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'MD2 microdiffractometer with MK3 mini-kappa'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_collimation    'Rh-coated Si focusing mirrors'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.76000
_diffrn_reflns_av_R_equivalents  0.1182
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6040
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        14.857
_diffrn_reflns_theta_max         14.857
_diffrn_reflns_theta_min         2.174
_diffrn_source                   synchrotron
_diffrn_source_type              'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.5770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1163 before and 0.0915 after correction. The Ratio of minimum to maximum transmission is 0.7757. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             1106
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.7757
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+84.9111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2346
_refine_ls_wR_factor_ref         0.2839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1180
_reflns_number_total             1832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07766a2.cif
_cod_data_source_block           mo_tr_nitppp2_0m_pl
_cod_depositor_comments          'Adding full bibliography for 7120965.cif.'
_cod_original_formula_sum        'C45.50 H24 N4 Ni2 O14 P4'
_cod_database_code               7120965
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C2(0.66) H2(0.66) C3(0.66) H3(0.66) C46(0.34) H46(0.34) C45(0.34)
 H45(0.34) C47(0.5)
3.a Riding coordinates:
 C46(H46), C45(H45)
3.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C30(H30), C31(H31), C33(H33), C34(H34), C20(H20), C19(H19),
 C22(H22), C23(H23), C25(H25), C26(H26), C38(H38), C39(H39), C41(H41), C42(H42),
  C35(H35), C2(H2), C3(H3), C43(H43), C44(H44), C27(H27), C28(H28), C8(H8),
 C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'