Cr(III)-HMC (HMC = 5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane) Alkynyl Complexes: Preparation and Emission Properties.
Tyler, Sarah F.; Judkins, Eileen C.; Song, You; Cao, Fan; McMillin, David R.; Fanwick, Phillip E.; Ren, Tong; Inorganic chemistry 55 (2016) 8736–8743; doi:10.1021/acs.inorgchem.6b01285

data_4348513
_publ_section_title
;
 Cr(III)-HMC (HMC =
 5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane) Alkynyl
 Complexes: Preparation and Emission Properties.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8736
_journal_page_last               8743
_journal_paper_doi               10.1021/acs.inorgchem.6b01285
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C30 H54 Cr1 N4 Si2,Cl1'
_chemical_formula_sum            'C30 H54 Cl Cr N4 Si2'
_chemical_formula_weight         614.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2089(5)
_cell_length_b                   12.8204(5)
_cell_length_c                   22.5411(14)
_cell_measurement_reflns_used    13083
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.000
_cell_measurement_theta_min      5.374
_cell_volume                     3528.2(3)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13083
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         5.374
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    4.184
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00067(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+6.7869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2137
_reflns_number_total             3069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01285_si_002.cif
_cod_data_source_block           SFTCR4
_cod_database_code               4348513
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.488
_shelx_estimated_absorpt_t_max   0.554
_shelx_res_checksum              67746
_shelx_hkl_checksum              36598