The Big Impact of a Small Detail: Cobalt Nanocrystal Polymorphism as a Result of Precursor Addition Rate during Stock Solution Preparation
Nikos Liakakos; Benoît Cormary; Xiaojian Li; Pierre Lecante; Marc Respaud; Laurent Maron; Andrea Falqui; Alessandro Genovese; Laure Vendier; Spyros Koïnis; Bruno Chaudret; Katerina Soulantica; Journal of the American Chemical Society 134 (2012) 17922–17931; doi:10.1021/ja304487b

data_4118839
_publ_contact_author
;
Katerina Soulantica
;
_publ_contact_author_address
;
Universit\'e de Toulouse
INSA, UPS, CNRS, LPCNO
135 avenue de Rangueil
31077 Toulouse, France
;
_publ_contact_author_email       Katerina.Soulantika@insa-toulouse.fr
_publ_section_title
;
 The Big Impact of a Small Detail: Cobalt Nanocrystal Polymorphism as a
 Result of Precursor Addition Rate during Stock Solution Preparation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17922
_journal_page_last               17931
_journal_paper_doi               10.1021/ja304487b
_journal_volume                  134
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H52 Co N2 O4'
_chemical_formula_sum            'C24 H52 Co N2 O4'
_chemical_formula_weight         491.61
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   51.020(10)
_cell_length_b                   5.7091(11)
_cell_length_c                   9.941(2)
_cell_measurement_reflns_used    2200
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.998
_cell_measurement_theta_min      3.0297
_cell_measurement_wavelength     0.71073
_cell_volume                     2886.5(10)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_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      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.1152438535
_diffrn_orient_matrix_UB_12      0.0189249592
_diffrn_orient_matrix_UB_13      -0.0099138191
_diffrn_orient_matrix_UB_21      0.0336910271
_diffrn_orient_matrix_UB_22      0.0690023641
_diffrn_orient_matrix_UB_23      0.0043220772
_diffrn_orient_matrix_UB_31      0.0348779228
_diffrn_orient_matrix_UB_32      -0.0018622921
_diffrn_orient_matrix_UB_33      -0.0257108435
_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  0.1226
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9868
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.255
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.38
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                1880
_reflns_number_total             2717
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja304487b_si_002.cif
_cod_data_source_block           cat170106
_cod_database_code               4118839