Effect of a methyl group on the spontaneous resolution of a square-pyramidal coordination compound: crystal packing and conglomerate formation
Biswas, Apurba; Estarellas, Carolina; Frontera, Antonio; Ballester, Pablo; Drew, Michael G. B.; Gamez, Patrick; Ghosh, Ashutosh; CrystEngComm 14 (2012) 5854–; doi:10.1039/c2ce25497b

data_7214641
_publ_section_title
;
 Effect of a methyl group on the spontaneous resolution of a
 square-pyramidal coordination compound: crystal packing and conglomerate
 formation
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              5854
_journal_paper_doi               10.1039/c2ce25497b
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C18 H23 Cu N3 O3'
_chemical_formula_weight         392.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 103.643(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.126(5)
_cell_length_b                   13.963(5)
_cell_length_c                   14.834(5)
_cell_measurement_reflns_used    23296
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.03
_cell_volume                     1836.9(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23296
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.7599
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0539P)^2^+0.1876P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                3635
_reflns_number_total             4633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25497b.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7214641