Synthetic, spectroscopic, and structural studies on organoimido molybdenum, tungsten, and rhenium phthalocyanines.
Darwish, Wael; Seikel, Elisabeth; Harms, Klaus; Burghaus, Olaf; Sundermeyer, Jörg; Dalton transactions (Cambridge, England : 2003) 40 (2011) 1183–1188; doi:10.1039/c0dt01166e

data_7014794
_publ_section_title
;
 Synthetic, spectroscopic, and structural studies on organoimido
 molybdenum, tungsten, and rhenium phthalocyanines.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1183
_journal_page_last               1188
_journal_paper_doi               10.1039/c0dt01166e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C36 H25 Cl Mo N9, 7(H2 O)'
_chemical_formula_sum            'C36 H39 Cl Mo N9 O7'
_chemical_formula_weight         841.15
_chemical_name_systematic        ?
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8148(12)
_cell_length_b                   13.8148(12)
_cell_length_c                   10.0926(9)
_cell_measurement_reflns_used    8979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      1.47
_cell_volume                     1926.2(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'DIAMOND 3.2 (Crystal Impact)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0492
_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       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12104
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.9432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]

;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1702
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0387P)^2^+1.4570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                1424
_reflns_number_total             1702
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0DT01166E.TXT
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7014794