Vapour- and solvent-mediated crystalline transformations in Mo(vi) hydrazone complexes controlled by noncovalent interactions
Mandarić, Mirna; Prugovečki, Biserka; Cvijanović, Danijela; Vuković, Jelena Parlov; Lovrić, Jasna; Skočibušić, Mirjana; Odžak, Renata; Cindrić, Marina; Vrdoljak, Višnja; CrystEngComm 21 (2019) 6281–; doi:10.1039/C9CE01273G

data_7234208
_publ_section_title
;
 Vapour- and solvent-mediated crystalline transformations in Mo(vi)
 hydrazone complexes controlled by noncovalent interactions
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              6281
_journal_paper_doi               10.1039/C9CE01273G
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C15 H15 Mo N3 O6'
_chemical_formula_weight         429.24
_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_method           SHELXL-2017/1
_audit_update_record
;
2019-07-29 deposited with the CCDC.    2019-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.424(3)
_cell_angle_beta                 76.154(4)
_cell_angle_gamma                89.268(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6639(4)
_cell_length_b                   9.7687(4)
_cell_length_c                   11.6636(4)
_cell_measurement_reflns_used    7078
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.9160
_cell_measurement_theta_min      4.5100
_cell_volume                     823.28(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;      
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13777
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         4.203
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.90887
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0270P)^2^+0.3216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3246
_reflns_number_total             3580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01273g2.cif
_cod_data_source_block           shelx_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7234205--7234213.cif.'
_cod_database_code               7234208
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              6181