Bis(triphenylphosphine)iminium Nitrito(phthalocyaninato)zincate Hydrate
Assmann, B.; Sievertsen, S.; Homborg, H.; Acta Crystallographica Section C 52 (1996) 876–879; doi:10.1107/S0108270195014351

data_2004760
_publ_section_title
;
 Bis(triphenylphosphine)iminium Nitrito(phthalocyaninato)zincate
 Hydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              876
_journal_page_last               879
_journal_paper_doi               10.1107/S0108270195014351
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac
'(C36 H30 N P2)[Zn (N O2) (C32 H16 N8)], H2 O1'
_chemical_formula_structural     ^b^(PNP)[Zn(ONO)Pc^2-^].H~2~O
_chemical_formula_sum            'C68 H48 N10 O3 P2 Zn'
_chemical_formula_weight         1180.47
_chemical_name_common
;
Bis(triphenylphosphine)iminiumnitrito(phthalocyaninato)zincate Hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                67.357(10)
_cell_angle_beta                 85.069(12)
_cell_angle_gamma                86.429(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6439(15)
_cell_length_b                   13.677(2)
_cell_length_c                   17.107(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      16.1
_cell_measurement_theta_min      4.2
_cell_volume                     2718.8(7)
_computing_cell_refinement       CAD-4/PC
_computing_data_collection       'CAD-4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      208(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 Turbo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7941
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         .345
_refine_diff_density_min         -.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment
;
Coordinates and U~iso~ of the H atoms of the hydrate refined; H atoms of the
phthalocyanine and (PNP)^+^ cation idealized (riding model)
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         7540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_obs          0.0295
_refine_ls_shift/esd_max         0.138
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0370P)^2^ + 1.6713P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0776
_refine_ls_wR_factor_obs         0.0726
_reflns_number_observed          6404
_reflns_number_total             7540
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1091.cif
_cod_data_source_block           ZnONO
_cod_original_cell_volume        2718.9(6)
_cod_database_code               2004760